반응 #1929074

반응 방정식

hydrochloric acid

compound

Methyl 1-{[(5-bromo-2-methylphenyl)acetyl]amino}-4,4-difluorocyclohexanecarboxylate

DMA

DMA

potassium tert-butoxide

→

3-(5-Bromo-2-methylphenyl)-8,8-difluoro-4-hydroxy-1-azaspiro[4.5]dec-3-en-2-one

용매

water

반응 조건

후처리

1. 1
   여과the resulting precipitate was filtered off with suction
2. 2
   세척washed with water
3. 3
   기타dried in a vacuum
4. 4
   기타drying cabinet at 50° C
5. 5
   workup.ADDITIONn-hexane was added
6. 6
   여과the mixture was filtered off with suction
7. 7
   기타dried

실험 절차

11.0 g (27.2 mmol) of the compound from Example 10A were initially charged in a solution of 22 ml of DMA (N,N-dimethylacetamide), a solution of 10 ml of DMA and 3.54 g (1.1 eq.) of potassium tert-butoxide was added dropwise at 20-30° C. and the mixture was stirred at 30° C. for a further 1 h. The mixture was poured into 200 ml of water and the mixture was adjusted to pH 2 using aqueous 1N hydrochloric acid, the resulting precipitate was filtered off with suction, washed with water and dried in a vacuum drying cabinet at 50° C. The product was suspended in hot methyl tert-butyl ether, n-hexane was added and the mixture was filtered off with suction and dried. This gave 11.0 g (97% of theory) of the title compound in a purity of 89%.

출처