تفاعل #1929081
ord-f0c18b8a86a34e51ad1a36a4a3bf9cda
معادلة التفاعل
hydrochloric acid
compound
Methyl 4,4-difluoro-1-{[(4′-fluoro-4-methylbiphenyl-3-yl)acetyl]amino}cyclohexanecarboxylate
DMA
DMA
potassium tert-butoxide
→
title compound
8,8-Difluoro-3-(4′-fluoro-4-methylbiphenyl-3-yl)-4-hydroxy-1-azaspiro[4.5]dec-3-en-2-one
المتفاعلات
الكواشف
لا شيء
المذيبات
ظروف التفاعل
الظروف التفصيلية
See reaction.notes.procedure_details.
المعالجة
- 1ترشيحthe resulting residue was filtered off with suction
- 2أخرىPurification by flash column chromatography (silica gel; ethyl acetate/n-hexane 1:1)
الإجراء التجريبي
2.80 g (5.94 mmol) of the compound from Example 7A were initially charged in a solution of 8 ml of DMA (N,N-dimethylacetamide), a solution of 5 ml of DMA and 1.75 g (2.5 eq.) of potassium tert-butoxide was added dropwise at 20° C. and the mixture was stirred at room temperature for 4 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 1:1) gave 1.07 g (44% of theory) of the title compound.