HRID1253839
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- additionThe reaction mixture is poured on ice-water
- extractionextracted with CH2Cl2
- customAfter the usual work-up the residue is purified over silica gel on a glass
- filtrationfilter (eluent: CH2Cl2/MeOH=98:2)