- Improved method used for preparing quinazoline drugs
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The invention relates to an improved method used for preparing quinazoline drugs, and provides a synthesis route taking 2-chloro-4-amino-6,7-dimethoxyquinazoline as an intermediate. The synthesis route comprises following steps: acrylonitrile and a methylamine alcohol solution are subjected to amination reaction so as to obtain intermediate (I); triethylamine is taken as an acid binding agent, andbenzyl chloride is taken as a protective group so as to obtain an intermediate (II); a metal hydride is adopted so as to obtain an intermediate (III) through reduction; acylation with tetrahydro-2-furancarbonylchloride is carried out so as to obtain an intermediate (IV); the intermediate (IV) and ammonium formate are subjected to hydrogenolysis under catalytic effect of palladium on carbon so asto obtain an intermediate (V); and at least condensation reaction with 2-chloro-4-amino-6,7-dimethoxyquinazoline is carried out so as to obtain quinazoline drug Alfuzosin Hydrochloride (VI). Comparedwith the prior art, the improved method possesses following advantages: operation is simple and safe; reaction conditions are convenient to control; energy consumption is low; yield is stable; and industrialized application prospect is promising.
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Paragraph 0032; 0035
(2018/07/06)
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- A process for the preparation of alfuzosin hydrochloride method (by machine translation)
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The invention relates to a process for the preparation of alfuzosin hydrochloride method, method comprises the following steps: (1) 15 °C following, acrylonitrile into the the methylamine is mellow solution to stir, by distillation to obtain (I); (2) to (I) is dripped reducing agent in an organic solvent, heating to reflux, then slowly sequentially into the 25% sodium hydroxide solution and distilled water, by the distillation treatment to obtain the (II); (3) under dry condition, the thionyl chloride is slowly dripped into the 2 - tetrahydrofuran formic acid, a 2 - tetrahydrofuran chloride; (4) the temperature control in the 5 - 15 °C conditions, will be 2 - tetrahydrofuran formyl the chlorine drips into containing acid, organic solvent and (II) of the mixed solution, then completing the stirring 3 hours, for 25% sodium hydroxide solution to neutralize, by organic solvent extraction, (III) be; (5) to (III) with 2 - chloro - 4 - amino - 6, 7 - dimethoxy quinazoline in presence of organic solvent, reflux stirring 4 - 10 hours, cooling and filtering, and steaming and removing the organic solvent, acetone dispersed precipitate solid, then re-crystallizing mixed solvent, to get the alfuzosin hydrochloride (IV). (by machine translation)
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Paragraph 0023; 0024; 0025
(2017/08/29)
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- Amine composition
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The present invention provides novel polymeric amine compositions employing amine compounds having multiple tertiary amine groups. Methods of making these new compositions are also disclosed. Amine compositions and amine-epoxy compositions employing the polymeric amine compositions of the present invention are also provided.
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Page/Page column 21
(2015/10/28)
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- Autocatalytic polyols
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The present invention provides polymeric polyol compositions employing polyol compounds having multiple tertiary amine groups. Methods of making these compositions are also disclosed. Polyol formulations containing these polymeric polyol compositions and methods of making polyurethane gel and foam employing such polymeric polyol compositions are also provided.
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Paragraph 0208; 0209; 0210; 0211
(2013/03/26)
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- Synthesis of a novel ionic liquid with both Lewis and Br?nsted acid sites and its catalytic activities
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The novel ionic liquid with both Lewis and Br?nsted acid sites has been synthesized and its catalytic activities for acetalization and Michael addition were investigated carefully. The novel ionic liquid was stable to water and could be used in aqueous solution. Furthermore, the molar ratio of the Lewis and Br?nsted acid sites could be adjusted according to different reactions. The results showed that the novel ionic liquid was very efficient for the traditional acid-catalyzed reactions with good to excellent yields in short time.
- Liang, Xuezheng,Qi, Chenze
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experimental part
p. 808 - 812
(2012/01/04)
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- Novel efficient procedure for the conjugate addition of amines to electron deficient alkenes
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The novel efficient procedure has been developed for the conjugate addition of amines to electron deficient alkenes using the novel SO3H functionalized ionic liquid as catalyst. The results showed that the novel catalyst owned high activities for the reactions with excellent yields within several minutes. Various amines and electron deficient alkenes were successfully transformed to the corresponding products in the catalytic system. Operational simplicity, without need of any solvent, low cost of the catalyst used, room temperature, high yields, reusability, excellent chemoselectivity and wide applicability are the key features of this methodology.
- Sun, Xudong,Du, Yijun,Li, Chunqing,Qi, Chenze
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experimental part
p. 653 - 656
(2011/02/16)
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- Novel synthesis of 3-aminopropionitriles by ring opening of 2-oxazolidinones with cyanide ion
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Nucleophilic attack of cyanide ion on the 5-position of 2-oxazolidinones in the presence of 18-crown-6 gave 3-aminopropionitriles.
- Taniguchi, Tsuyoshi,Goto, Naoya,Ishibashi, Hiroyuki
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supporting information; experimental part
p. 4857 - 4858
(2009/10/26)
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- SUBSTITUTED QUINAZOLINE DERIVATIVES AND THEIR USE AS INHIBITORS
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The use of a compound of formula (I) 1 or a salt, ester or amide thereof; where X is O, or S, S(O) or S(O)2, or NR6 where R6 is hydrogen or C1-6 alkyl,; R5 is an optionally substituted 5-membered heteroaromatic ring, R1, R2 ,R3, R4 are independently selected from various specified moieties, in the preparation of a medicament for use in the inhibition of aurora 2 kinase. Certain compounds are novel and these, together with pharmaceutical compositions containing them are also described and claimed
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- Scavenger assisted combinatorial process for preparing libraries of amides, carbamates and sulfonamides
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This invention relates to a novel solution phase process for the preparation of amide, carbamate, and sulfonamide combinatorial libraries. These libraries have utility for drug discovery and are used to form wellplate components of novel assay kits.
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- Synthesis of pyrroloazepines. Facile synthesis of 2-substituted pyrrole derivatives by the phosgene method
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A highly convenient method for the synthesis of 2-substituted pyrrole derivatives 7a-c from pyrrole using phosgene was developed. Successively, 7-methyl-6,7-dihydro-1H,5H-pyrrolo[2,3-c]azepine-4,8-dione 1a and 6,7-dihydro-1H,5H-pyrrolo[2,3-c]azepine-4,8-dione 1b (aldisin) were synthesized by phosphorus pentoxide/methanesulfonate and polyphosphoric acid cyclization.
- Cho, Hidetsura,Matsuki, Shinsuke,Mizuno, Akira,Annoura, Hirokazu,Tatsuoka, Toshio
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- Amino disazo dyestuffs containing a fluoropyrimidinyl or a fluorotriazinyl reactive group
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Dyestuffs of the formula STR1 wherein X=--CH=CH2, --CH2 --CH2 OSO3 H, --CH=CHCl or --CH2 --CH2 Cl and Y=a fiber-reactive fluoropyrimidinyl or fluorotriazine radical and wherein u and v=H or SO3 H, where u~v. Such dyestuffs suitable for dyeing and printing diverse substrates, particularly cotton, to give products a high degree of dyestuff fixation.
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- Nucleoside Syntheses, XXI. Synthesis of 5-Methylaminomethyl-2-thiouridine, a Rare Nucleoside from t-RNA
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The synthesis of 5-methylaminomethyl-2-thiouridine (1), a rare nucleoside from t-RNA, starting from the appropriate 2-thiouracil and ribose derivatives is described.During the silyl Hilbert-Johnson nucleoside synthesis with silver perchlorate the tert-butoxycarbonyl (Boc) aminoprotecting group in the 2-thiouracil moiety is removed.This cleavage is due to the intermediate formation of trimethylsilyl perchlorate.Preparative applications of this new type of Lewis acids are mentioned.
- Vorbrueggen, Helmut,Krolikiewicz, Konrad
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p. 1438 - 1447
(2007/10/02)
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