반응 #1929083

반응 방정식

hydrochloric acid

compound

Methyl 1-{[(4′-chloro-2,4-dimethylbiphenyl-3-yl)acetyl]amino}-4,4-difluorocyclohexanecarboxylate

DMA

DMA

potassium tert-butoxide

→

title compound

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

용매

water

반응 조건

후처리

1. 1
   여과the resulting residue was filtered off with suction
2. 2
   기타Purification by flash column chromatography (silica gel; ethyl acetate/n-hexane 2:1)

실험 절차

2.55 g (5.29 mmol) of the compound from Example 9A were initially charged in a solution of 5 ml of DMA (N,N-dimethylacetamide), a solution of 5 ml of DMA and 1.88 g (3 eq.) of potassium tert-butoxide was added dropwise at 20° C. and the mixture was stirred at room temperature for 24 h. The mixture was poured into 200 ml of water and the reaction was adjusted to pH 2 using concentrated aqueous hydrochloric acid, and the resulting residue was filtered off with suction. Purification by flash column chromatography (silica gel; ethyl acetate/n-hexane 2:1) gave 0.87 g (31% of theory) of the title compound.

출처