HRID22277

反应详情

EQUATION

反应方程式

HRID 22277 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To 2,6-bis (1,1-dimethylethyl)-4-(N-methyl-N-[1-phenyl-1H-pyrazol-3-yl]amino)phenol (0.6 g) in dry tetrahydrofuran (15 ml) at -78° under nitrogen was added butyl lithium (1.29 ml of 1.4M hexane solution). After 10 minutes acetyl chloride (0.2 ml) was added. The reaction was left for 16 hours, poured into water and extracted with ethyl acetate. Evaporation, and chromatography (silica, dichloromethane/hexane [1:1]) of the residue, followed by recrystallisation from hexane at -20° gave the title compound (0.35 g), mp 102°-103°.

WORKUP

后处理

  1. extractionextracted with ethyl acetate
  2. customEvaporation, and chromatography (silica, dichloromethane/hexane [1:1]) of the residue
  3. customfollowed by recrystallisation from hexane at -20°