HRID2243869

反应详情

EQUATION

反应方程式

HRID 2243869 的结构方程式

CONDITIONS

反应条件

温度
58 °C

PROCEDURE

实验过程

A solution of tert-butyl 7-(4-(allyloxy)phenyl)-5-oxo-9-oxa-2-thia-4,8-diazaundec-7-en-3-ylidenecarbamate from Step D (1.14 g) in THF (4 mL) was added 4-(aminomethyl)-2,6-dichloroaniline (647 mg) and diisopropylethylamine (0.46 mL), and the resulting mixture was heated at 58° C. for 12 h. The solvents were removed in vacuo, and the residue was purified by Biotage eluting with 10-25% ethyl acetate/90-75% hexanes to give the title compound as a yellowish oil (1.28 g). retention time: 2.37 min (method A). MS (ESI) (M+H)+ 578.23.

WORKUP

后处理

  1. customThe solvents were removed in vacuo
  2. customthe residue was purified by Biotage
  3. washeluting with 10-25% ethyl acetate/90-75% hexanes