反应详情

To a mixture of (2-amino-4,5-difluoro-phenyl)-carbamic acid tent-butyl ester (1.00 g, 4 mmol, 1.0 equiv) and (S)-alpha-methoxyphenylacetic acid (0.68 g, 1.0 equiv., [CAS RN 26164-26-1]) in methanol (25 mL) were added cyclohexanecarbaldehyde (0.459 g, 4 mmol, 1.0 equiv; [2043-61-0]) and benzyl isonitrile (0.48 g, 1.0 equiv., 4 mmol, CAS RN 10340-91-7). The mixture was stirred overnight at room temperature. A solution of 4 M HCl in dioxane (3 mL) was added, and the reaction mixture stirred at room temperature overnight. The mixture was partitioned between water (100 ml) and ethyl acetate (100 ml). The phases were separated and the aqueous phase extracted with ethyl acetate (2×50 ml), the combined organic phases washed with brine, dried over sodium sulfate and evaporated under reduced pressure to afford the title compound as an orange gum (2.16 g, quant., mixture of diastereomers) that was used without further purification. MS (ISP): 504.1 [M+H]+.

1. stirringthe reaction mixture stirred at room temperature overnight
2. customThe mixture was partitioned between water (100 ml) and ethyl acetate (100 ml)
3. customThe phases were separated
4. extractionthe aqueous phase extracted with ethyl acetate (2×50 ml)
5. washthe combined organic phases washed with brine
6. dry with materialdried over sodium sulfate
7. customevaporated under reduced pressure