HRID469302

反应详情

EQUATION

反应方程式

HRID 469302 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
-75 °C

PROCEDURE

实验过程

Under an argon atmosphere 2.8 mL (4.5 mmol) of a 1.6 M n-butyllithium solution were added to a mixture of 1.2 g (4.0 mmol) 2-benzyloxy-5-bromo-1,3-dimethyl-benzene in mL THF cooled to −75° C. and the mixture was stirred for 1 h at −75° C. Then 0.96 g (4.3 mmol) 6-chloro-pyrimidine-4-carboxylic acidmethoxy-methyl-amide, dissolved in 10 mL THF, were added dropwise. After another 30 min stirring at −75° C. the reaction mixture was slowly heated to 0° C. The mixture was combined with saturated sodium hydrogen carbonate solution and extracted with diethyl ether. The organic phase was dried and evaporated down. The residue was purified by flash chromatography.

WORKUP

后处理

  1. additionwere added dropwise
  2. stirringAfter another 30 min stirring at −75° C. the reaction mixture
  3. temperaturewas slowly heated to 0° C
  4. extractionextracted with diethyl ether
  5. customThe organic phase was dried
  6. customevaporated down
  7. customThe residue was purified by flash chromatography