HRID2267351

反应详情

EQUATION

反应方程式

HRID 2267351 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
180 °C

PROCEDURE

实验过程

1.22 mL (0.71 mmol) of a 10% (w/v) solution of 1-(2-aminoethyl)-5,5-dimethylimidazol-idine-2,4-dione in MeOH was added to a 10 mL microwave vessel. The MeOH was evaporated with a stream of N2, to leave an oily solid which was dissolved in 0.34 mL (2.0 mmol) of N,N-diisopropylethylamine, 0.5 mL of N-methylpyrrolidinone and 3.5 mL of toluene, to which was added 0.15 g (0.65 mmol) of 4-(5-bromothiophen-2-yl)-2-chloropyrimidine. The reaction solution was heated in a microwave to 180° C. for 20 min then concentrated in vacuo and purified by flash chromatography eluting with a linear gradient of 75% EtOAc in hexane to neat EtOAc to deliver The title compound. MS (M+H)+ 410.

WORKUP

后处理

  1. customThe MeOH was evaporated with a stream of N2
  2. customto leave an oily solid which
  3. concentrationthen concentrated in vacuo
  4. custompurified by flash chromatography
  5. washeluting with a linear gradient of 75% EtOAc in hexane to neat EtOAc