HRID930290

反应详情

EQUATION

反应方程式

HRID 930290 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 5-chloro-N-((4S,6S)-4-(5-(5-chloropicolinamido)-2-fluorophenyl)-4-methyl-6-(trifluoromethyl)-5,6-dihydro-4H-1,3-oxazin-2-yl)picolinamide (4k 85.3 mg, 0.150 mmol) in 2 M NH3/MeOH (Aldrich; 4.0 mL) was heated to 50° C. for 16 h. The solution was concentrated and purified by flash chromatography on silica gel (Gradient: 20%→100% EtOAc/hexane) to give the title compound (48.2 mg, 0.112 mmol) as a white solid. MS m/z=431.0, [M+H]+. Calculated for C18H15ClF4N4O2: 430.8

WORKUP

后处理

  1. concentrationThe solution was concentrated
  2. custompurified by flash chromatography on silica gel (Gradient: 20%→100% EtOAc/hexane)