HRID584684
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
CONDITIONS
反应条件
- 温度
- 200 °C
PROCEDURE
实验过程
A mixture of 2-bromoaniline (2.18 g, 12.7 mmol) and 2,3-diphenylmaleic anhydride (3.17 g, (12.7 mmol) were stirred and heated under argon to 200° C. for 6 h. The mixture was cooled to room temperature, dissolved in CH2Cl2 (50 mL), dried (MgSO4) and evaporated. Purification of the crude product by flash chromatography on silica gel (5×25 cm column, 2 L of 3:7 hexanes/CH2Cl2, then CH2Cl2) gave first 4-(2-bromoanilino)-2,3-diphenyl-4-hydroxybutyrolactone (2.16 g, 40% yield) as a yellow solid, mp 162-164° C. and then the title compound as a bright yellow solid, mp 178-180° C., 2.00 g, 39% yield.
WORKUP
后处理
- temperatureThe mixture was cooled to room temperature
- dry with materialdried (MgSO4)
- customevaporated
- customPurification of the crude product by flash chromatography on silica gel (5×25 cm column, 2 L of 3:7 hexanes/CH2Cl2