HRID1257744

反应详情

EQUATION

反应方程式

HRID 1257744 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To the reaction mixture from the above step containing (1R,3R)-3-(1-Benzenesulfonyl-5-nitro-1H-pyrrolo[2,3-b]pyridin-4-ylamino) cyclohexanol (8.65 mmol) in isopropyl alcohol (30 mL) was added 10% Palladium on activated carbon (718 mg). The reaction mixture was then capped with a 3 way glass valve with a hydrogen gas balloon. The flask was opened to vacuum for two minutes, followed by opening to hydrogen. This purge/flush cycle was repeated 3 times before stirring under a hydrogen atmosphere at room temperature for 2 days. LC/MS showed that the reaction went to completion. The reaction mixture was then filtered through celite 545 and concentrated to give a black foamy solid, which was used as is for the next step. LCMS (Method M, ESI): RT=1.44 min, m+H=386.8.

WORKUP

后处理

  1. filtrationThe reaction mixture was then filtered through celite 545
  2. concentrationconcentrated
  3. customto give a black foamy solid, which