反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
CONDITIONS
反应条件
- 温度
- 180 °C
PROCEDURE
实验过程
(S)-methyl 3-(5-chloropyridin-2-yl)-3-(3-fluoro-5-(trifluoromethyl)phenyl)-3-((R)-2-methylpropan-2-ylsulfinamido)propanoate (0.10 g, 0.20 mmol) was dissolved in 8N NH3 solution in ethylene glycol (1 mL) in a microwave vial. The reaction mixture was heated to 180° C. for 300 sec, the pressure was cautiously vented and the reaction mixture purified directly by prep HPLC (YMC ODSA30×100 mm, 0-100% over 10 min, MeOH/H2O/0.1% TFA). (S)-3-(5-chloropyridin-2-yl)-3-(3-fluoro-5-(trifluoromethyl)phenyl)-3-((R)-2-methylpropan-2-ylsulfinamido)propanamide was isolated as a white solid (0.041 g, 41% yield) LCMS: 1.85 min [M+1] 466.1 (2 min gradient, MeOH/H2O 0.1% TFA). Starting material was also recovered (0.055 g, 55% recovered yield).
WORKUP
后处理
- customthe reaction mixture purified directly by prep HPLC (YMC ODSA30×100 mm, 0-100% over 10 min, MeOH/H2O/0.1% TFA)