79333-82-7Relevant academic research and scientific papers
Synthesis method of doxepin hydrochloride
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Paragraph 0044-0046; 0101-0106, (2021/11/03)
The invention relates to a synthetic method of doxepin hydrochloride. The method comprises the following steps: (1) phosphites react with 3 - chlorine -1 - (N, N - dimethyl) propylamine to obtain 3 - (N, N - dimethyl) propyl phosphate, or a salt thereof with hydrochloric acid to obtain 3 - (N, N - dimethyl) propyl phosphate hydrochloride. (2) Reaction of 3 - (N, N -dimethyl) propyl phosphate or its hydrochloride with 6, 11 -dihydrodibenzo [b, e] oxepin -11 - ketone under strong base conditions Wittig to obtain doxorubicin. (3) The multi-plug is subjected to salt formation reaction with hydrochloric acid to prepare the doxorubicin hydrochloride. In 1st-step reaction step, the yield of the alkyl phosphate product prepared by adopting the reaction is high, thereby ensuring the yield and purity of the final product hydrochloride. Compared with the prior art, the method has the advantages of simple process, low production cost, less process steps and the like.
Reduction of Amides to Amines under Mild Conditions via Catalytic Hydrogenation of Amide Acetals and Imidates
Kadyrov, Renat
, p. 185 - 191 (2018/11/23)
A simple and general protocol was developed for selective conversion of amides into amines. Amides were converted into amide acetals and imido esters by O-alkylation and then hydrogenated without isolation into amines under very mild reaction conditions over standard hydrogenation catalysts. Triethyloxonium tertafluoroborate, methyl trifluoromethanesulfonate, dimethyl sulfate and ethyl chloroformate were validated as alkylating agent. The synthetic utility of this approach was demonstrated by the selective carbonyl reduction of peptide groups. Carbonyl reduction of peptide group proceeds chemoselective without racemization of the neighboring chiral center. (Figure presented.).
Catalytic Hydrogenation for Producing Amines from Carboxylic Acid Amides, Carboxylic Acid Diamides, Di-, Tri-, or Polypeptides, or Peptide Amides
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Paragraph 185-186, (2016/10/11)
The present invention relates to a process for the preparation of amines, comprising the following steps: a. reaction of a (i) carboxylic acid amide of the general formula (I), or (ii) carboxylic acid diamide of the general formula (II), or (iii) di-, tri- or polypeptide, or (iv) peptide amide with carboxy-terminal amide function with an alkylating agent, b. addition of a hydrogenation catalyst to the reaction mixture in a molar ratio of from 1:10 to 1:100 000, based on carboxylic acid amide, carboxylic acid diamide, di-, tri- or polypeptide or peptide amide, c. reaction of the reaction mixture with hydrogen, where a hydrogen pressure of from 0.1 bar to 200 bar is established and where a temperature in a range of from 0° C. to 250° C. is established.
AMINATION REDUCTRICE D'ALDEHYDES PHOSPHONIQUES. Un Reexamen
Collignon, N.,Fabre, G.,Varlet, J. M.,Savignac, Ph.
, p. 81 - 86 (2007/10/02)
The reactivity of diethyl-2-oxo ethyl- and 3-oxo propylphosphonates with ammonia, methyl and dimethylamine at pH 7 in the presence of sodium cyanohydridoborate via reductive amination of the carbonyl group has been reexamined.Reactions of diethyl-2-oxoethyl- and 3-oxopropylphosphonates with ammonia give imino-bis-(alkylphosphonates); methyl and dimethylamine give monocondensation products thus permitting the synthesis of N-substituted aminoalkylphosphonates.
