반응 #1929079

반응 방정식

potassium tert-butoxide

compound

Methyl 1-{[(4′-chloro-3′-fluoro-4-methylbiphenyl-3-yl)acetyl]amino}-4,4-difluorocyclohexanecarboxylate

hydrogen chloride

→

3-(4′-Chloro-3′-fluoro-4-methylbiphenyl-3-yl)-8,8-difluoro-4-hydroxy-1-azaspiro[4.5]dec-3-en-2-one

용매

N,N-dimethylformamide

반응 조건

후처리

1. 1
   workup.ADDITIONwas added dropwise until a pH of 1-2
2. 2
   workup.STIRRINGthe mixture was stirred for 30 minutes
3. 3
   여과filtered off with suction
4. 4
   세척the filter cake was washed with water
5. 5
   기타the precipitate was dried
6. 6
   기타For further purification
7. 7
   workup.DISSOLUTIONthe product was dissolved in 1N aqueous sodium hydroxide solution
8. 8
   기타precipitated by acidification with aqueous 1 N hydrochloric acid
9. 9
   workup.STIRRINGstirred for 30 minutes
10. 10
    세척washed with water
11. 11
    여과filtered off
12. 12
    기타dried

실험 절차

Under nitrogen, 2.23 g (19.9 mmol) of potassium tert-butoxide were added to 8.19 g (18.0 mmol) of the compound from Example 5A in 80 ml of N,N-dimethylformamide. The reaction mixture was stirred at room temperature for 15 minutes. The reaction mixture was then added to ice-water, 1N aqueous hydrogen chloride solution was added dropwise until a pH of 1-2 had been reached, the mixture was stirred for 30 minutes and filtered off with suction, the filter cake was washed with water and the precipitate was dried. For further purification, the product was dissolved in 1N aqueous sodium hydroxide solution, precipitated by acidification with aqueous 1 N hydrochloric acid, stirred for 30 minutes, washed with water, filtered off and dried. This gave 7.50 g (97% of theory) of the title compound.

출처