HRID731934

反应详情

EQUATION

反应方程式

HRID 731934 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To 2.00 g of 1-methylsulfonyl-6-nitroindoline and a mixed solvent of 100 ml of ethanol and 100 ml of tetrahydrofuran was added 300 mg of 10% palladium/carbon under an argon atmosphere, followed by 3 hours of stirring at room temperature under a hydrogen atmosphere. The reaction solution was filtrated through celite and the organic solvent in the filtrate was removed under reduced pressure. To the residue was added 200 ml of a mixed solution of methanol, ethyl acetate, and tetrahydrofuran. Under an argon atmosphere, 1 g of 10% palladium/carbon was added and the whole was stirred at room temperature for 3 hours under a hydrogen atmosphere. The reaction solution was filtrated through celite and the organic solvent in the filtrate was removed under reduced pressure to obtain 1.66 g of 1-methylsulfonyl-6-aminoindoline as a pale yellow solid.

WORKUP

后处理

  1. filtrationThe reaction solution was filtrated through celite
  2. customthe organic solvent in the filtrate was removed under reduced pressure
  3. additionTo the residue was added 200 ml of a mixed solution of methanol, ethyl acetate, and tetrahydrofuran
  4. additionUnder an argon atmosphere, 1 g of 10% palladium/carbon was added
  5. stirringthe whole was stirred at room temperature for 3 hours under a hydrogen atmosphere
  6. filtrationThe reaction solution was filtrated through celite
  7. customthe organic solvent in the filtrate was removed under reduced pressure