The method of obtaining 4,1'6'-trichloro-4,1',6'- trimethoxybenzoate

 

4,1', 6'-Trichloro-4,1', 6'-trimethoxybenzoate obtained by selective acetylation of sucrose in pyridine, chlorination obtained 6-monoacetylmorphine product in the provisions of 4,1', 6', paramilitary obtained in chlorinated pyridine and subsequent dezazetilirovanie and selection of the target product. From the reaction zone selective acetylation is removed by distillation with freezing the excess pyridine. Full acetate 4,1', 6'-trichloro-4,1', 6'-trimethoxybenzoate allocate by vicadine water. Dezazetilirovanie carried out with a solution of sodium methoxide in ethanol at room temperature for at least 4 h at pH 9, the resulting solution is neutralized, discolor and evaporated in vacuo to a dry residue. Chlorination lead suspension obtained by adding to the DMF petaluridae phosphorus. Processes for the preparation of suspensions and chlorination is carried out in a single reaction volume. The technical result is an increase in the yield of the target product. 2 C. p. F.-ly.

Tablicy

Claims

1. The method of obtaining 4,1’,6’-trichloro-4,1’,6’-deoxyglycosides on the basis of sucrose, including the electoral atsetilirovaniya obtained in chlorinated pyridine and subsequent dezazetilirovanie and selection of the target product, characterized in that the reaction zone selective acetylation is removed by distillation with freezing the excess pyridine, and received by paramilitaries full acetate 4,1’,6’-trichloro-4,1’,6’-deoxyglycosides allocate by vicadine water, dezazetilirovanie carried out with a solution of sodium methoxide in ethanol at room temperature for at least 4 h at pH 9, the resulting solution is neutralized, discolor and evaporated in vacuo to a dry residue.

2. Method p. 1, characterized in that the chlorination product selective acetylation lead suspension obtained by adding to the DMF petaluridae phosphorus under vigorous stirring and at a temperature below 20With, by adding a solution of 6-monoacetate sucrose in DMF at a temperature below 20C followed by warming the reaction mixture to 108-110C for no more than 2 hours and keeping at 108-110C for at least 1.5 hours

3. The method according to p. 2, characterized in that the preparation processes of the suspension and chlorination are in a single reaction volume.

 

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