HRID1507591

反应详情

EQUATION

反应方程式

HRID 1507591 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

CONDITIONS

反应条件

温度
90 °C

PROCEDURE

实验过程

To a suspension of 6-bromo-1-(3-cyclopropoxypropyl)-3,3-dimethylindolin-2-one (360 mg, 1.06 mmol) and K2CO3 (441 mg, 3.19 mmol) in DMSO (2 ml) were added L-proline (49.0 mg, 426 μmol), copper (I) iodide (40.5 mg, 213 μmol) and ammonium hydroxide (373 mg, 414 μl, 2.66 mmol). The tube was sealed and heated to 90° C. for 7 hours. The reaction mixture was poured into TBME (50 ml) and extracted with 1 M HCl. The combined aqueous layers were basified with 2M Na2CO3. The aqueous phase was extracted two times with TBME. The combined organic layers were dried over Na2SO4 and concentrated in vacuo. The title compound was obtained as brown viscous oil (228 mg).

WORKUP

后处理

  1. customThe tube was sealed
  2. extractionextracted with 1 M HCl
  3. extractionThe aqueous phase was extracted two times with TBME
  4. dry with materialThe combined organic layers were dried over Na2SO4
  5. concentrationconcentrated in vacuo