14602-86-9Relevant articles and documents
A convenient resolution method for 1,1′-bi-2-naphthol and 4,4′-dibromo-1,1′-spirobiindane-7,7′-diol with menthyl chloroformate in the presence of TBAB
Li, Zhian,Liang, Xinmiao,Wu, Fan,Wan, Boshun
, p. 665 - 669 (2004)
A convenient resolution method for 1,1′-bi-2-naphthol and 4,4′-dibromo-1,1′-spirobiindane-7,7′-diol has been developed with crude (-)-menthyl chloroformate as the resolution reagent in the presence of tetrabutylammonium bromide acting as a phase transfer catalyst in an aqueous NaOH/CH2Cl2 two phase solution. The deprotection of the hydroxy group was carried out via an aqueous KOH/EtOH solution. Both enantiomers of 1,1′-bi-2-naphthol and 4,4′-dibromo-1,1′- spirobiindane-7,7′-diol were obtained in high yields. Both ee's of (S)-(+) and (R)-(-)-4,4′-dibromo-1,1′-spirobiindane-7,7′-diol were above 99%. Most of the (-)-menthol could be easily recovered in a deprotection procedure and thus be reused for the formation of (-)-menthyl chloroformate without further purification.
Synthesis method of acetaldehyde alcohol optical active ester
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Paragraph 0024-0026, (2021/05/08)
The invention provides a synthesis method of an acetaldehyde alcohol optical active ester, which comprises the following steps of: reacting L-menthol as a raw material with triphosgene to obtain L-menthyl chloroformate, reacting the L-menthyl chloroformate with 1, 4-cis-butenediol, recrystallizing, and carrying out oxidation reaction under an ozone condition to obtain the acetaldehyde alcohol optical active ester. In the whole synthesis process, the initial raw materials are low in price and easy to obtain, the synthesis process is simple, the synthesis conditions are mild, and the synthesis cost of the acetaldehyde alcohol optical active ester is greatly reduced. The raw materials are good in reaction selectivity and high in atom utilization rate, and the obtained acetaldehyde alcohol optical active ester has high yield and purity. Meanwhile, few three-waste pollutants are generated in the synthesis process, and the method is suitable for industrial large-scale production of the acetaldehyde alcohol optical active ester, so that large-scale synthesis of drugs such as emtricitabine and lamivudine is facilitated.
PROCESS FOR PRODUCING CHLOROFORMATE COMPOUND
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Paragraph 0068; 0069; 0078, (2019/06/20)
The present invention provides a method for safely producing a large amount of chloroformate compound with high yield. The chloroformate compound can be produced by mixing and reacting a solution of triphosgene, an amine and an alcohol compound in a flow reactor. The chloroformate compound can also be produced by mixing and reacting a solution of triphosgene with a solution comprising an amine and an alcohol compound in a flow reactor. The amine is preferably tributylamine, and preferably used in an amount of 0.8 to 3 equivalents relative to an amount of the alcohol compound.
A Suitqable to preparation method
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Paragraph 0042; 0046-0048, (2019/04/02)
The invention discloses a Suitqable to preparation method. Refined pure 5 S - (5 '- fluorocytosine yl - 1') - 1, 3 - oxathiolane - 2 - ethoxy carbonyl - (1 'R, 2'S, 3' R) - menthyl ester; in the weak base and the solvent removed under the condition of chiral L - menthol get products Suitqable to. The invention required the starting raw material is cheap, mild reaction conditions, the atom utilization rate is high, the operation technique is simple, the reagents used in the environmental protection, the resulting high purity, reach the medical standard, is suitable for the industrial production of kindness or gemcitabine.
