HRID1474026
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
To a flask was added 2-chloro-5-(pyrimidin-2-ylamino)phenol (50 mg, 0.23 mmol), 4-methylpent-3-en-2-ol (23 mg, 0.23 mmol), Ph3P (59 mg, 0.23 mmol) and THF (0.08 mL). The reaction vessel was lowered into a sonication bath and sonicated for several minutes giving a clear and highly viscous solution. While sonication, DEAD (0.044 mL, 0.23 mmol) was added. After 1 h, the reaction mixture was concentrated in vacuo and the crude product was purified by flash chromatography on silica gel (hexane:EtOAc 7/3) to give the product in 17% yield (12 mg).
WORKUP
后处理
- customThe reaction vessel was lowered into a sonication bath
- customsonicated for several minutes
- customgiving a clear and highly viscous solution
- additionwas added
- concentrationthe reaction mixture was concentrated in vacuo
- customthe crude product was purified by flash chromatography on silica gel (hexane:EtOAc 7/3)
- customto give the product in 17% yield (12 mg)