HRID2079578

反应详情

EQUATION

反应方程式

HRID 2079578 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

Under nitrogen atmosphere, to a solution of {1-[7-(4-bromo-2,6-dimethylphenyl)-2,5-dimethyl-7H-pyrrolo[2,3-d]pyrimidin-4-yl]piperidin-4-yl}methanol (0.50 g) and 4-dimethylaminopyridine (0.55 g) in CH2Cl2 (50 mL) at 0° C. diethyl chlorophosphate (0.38 g) was added dropwise and the reaction is slowly heated up to room temperature. The reaction mixture is poured on ice-water and extracted with CH2Cl2. After the usual work-up the residue is purified over silica gel on a glass filter (eluent: CH2Cl2/MeOH=98:2) yielding product 3-017 (0.31 g).

WORKUP

后处理

  1. additionThe reaction mixture is poured on ice-water
  2. extractionextracted with CH2Cl2
  3. customAfter the usual work-up the residue is purified over silica gel on a glass
  4. filtrationfilter (eluent: CH2Cl2/MeOH=98:2)