Back to results
US 2006/0135789 A1Published application
Process for the preparation of gabalactam
AssigneeHikal Limited
InventorsNagarajan Kuppuswamy, Sivaramakrishnan Hariharan, Arulselvan Mariadas
Life of this patent
Estimating the term…
Abstract
This invention relates to an improved process for the preparation of gabalactum. Gabalactum is chemically known as 2-azaspiro(4,5)decan-3-one. Gabalactum has the structural formula 1 given.
Claims15
An improved process for the preparation of gabalactam of the formula 1
- Which comprises
- (i) Preparing an aqueous solution of an alkali or alkaline earth hydroxide in a concentration ranging from 10 to 20% by weight, adding bromine to the resulting solution to give the appropriate alkali or alkaline earth hypobromite solution having a concentration ranging from 5 to 10% by weight,
- (ii) adding 1 part by weight of an amide of the formula 4
- to 7.5 to 9.5 parts by weight, of the solution of the alkali/alkaline earth hypobromite obtained in step (i) during a period in the range of 1-4 hours, at a temperature in the range of −10 to +10 degrees C.,
- (iii) Keeping the resultant mixture for ageing in the temperature in the range of −10 to +10 degree C. for a period in the range of 0.5 to 2 hours,
- (iv) Heating the mixture gradually to a temperature in the range of 80 to 100 degrees C., for a period in the range of 3 to 8 hours,
- (v) Cooling the reaction mixture to a temperature in the range of 30 to 50 degrees C.,
- (vi) Extracting the mixture using a nonpolar solvent or a mixture thereof,
- (vii) subjecting the resulting organic layer washed aqueous layer to the steps of (iii) to (v) defined above
- (viii) Combining the organic layers obtained in steps ((vi) & (vii) together
- (ix) washing resulting combined organic layers with water at a temperature in the range of 30-35 and
- (x) Distilling of the organic solvent at a temperature in the range of 60-110 deg C., under reduced pressure.
9 more elements
Dependencies are inferred from the claim text.