HRID1442992
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
产物
AUXILIARIES
试剂、催化剂与溶剂
CONDITIONS
反应条件
- 温度
- 70 °C
PROCEDURE
实验过程
The crude tert-butyl (2R)-2-({[7-(benzyloxy)-4-chloroquinazolin-5-yl]oxy}methyl)-pyrrolidine-1-carboxylate was taken up in THF (5 ml) and 3-chloro-4-fluoroaniline (160 mg) and N,N-diisopropylethylamine (580 μl) were each added in one portion and the solution was heated at 70° C. for 18 hours. The reaction mixture was cooled to room temperature and concentrated in vacuo to leave a thick brown oil. Purification by flash chromatography, using 1.5% methanol in DCM as eluent, gave the tert-butyl (2R)-2-[({7-(benzyloxy)-4-[3-chloro-4-fluoroanilino]quinazolin-5-yl}oxy)methyl]pyrrolidine-1-carboxylate as a beige foam (350 mg, 54% over 2 steps); Mass spectrum MH+ 481.
WORKUP
后处理
- additioneach added in one portion
- temperatureThe reaction mixture was cooled to room temperature
- concentrationconcentrated in vacuo
- customto leave a thick brown oil
- customPurification by flash chromatography