HRID921851
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
Tert-butyl (2-chloro-5-cyano-3-(4-hydroxybut-1-en-2-yl)phenyl)carbamate (272 mg, 0.843 mmol) was taken up in EtOH (8 mL) and the flask was evacuated and filled with N2 3×. Next, platinum (IV) oxide (19.14 mg, 0.084 mmol) was added, and the flask was purged again. The reaction was stirred under 1 atm hydrogen at room temperature for 3 h. The reaction was monitored by TLC. The reaction mixture was filtered through celite, rinsing with MeOH. The solvent was removed in vacuo and the material was purified by flash column chromatography (0-40% EtOAc/Hex; 40 g column). Tert-butyl (2-chloro-5-cyano-3-(4-hydroxybutan-2-yl)phenyl)carbamate (161 mg) was obtained as a colorless glassy liquid.
WORKUP
后处理
- customthe flask was evacuated
- additionfilled with N2 3×
- customthe flask was purged again
- filtrationThe reaction mixture was filtered through celite
- washrinsing with MeOH
- customThe solvent was removed in vacuo
- customthe material was purified by flash column chromatography (0-40% EtOAc/Hex; 40 g column)