HRID12214

反应详情

EQUATION

反应方程式

HRID 12214 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

The crude N-(6-chloro-8-nitro-9H-β-carbolin-4-yl)-2,2,2-trifluoro-acetamide (130 mg, 0.36 mmol) was dissolved in 7 ml of MeOH and the reaction vessel was vacuum purged 3× with N2. Platinum (20 mg, 20% wt. on activated carbon) was added quickly, and the reaction vessel was again vacuum purged 3× with N2, followed by 3 additional vacuum purge cycles with H2. The reaction was allowed to stir under H2 at 1 atm overnight. Upon completion, the reaction vessel was purged of H2 and filtered over celite. The celite was washed several times with methanol until the filtrates were clear. The combined filtrates were concentrated to give N-(8-amino-6-chloro-9H-β-carbolin-4-yl)-2,2,2-trifluoro-acetamide as a yellow solid (112 mg, 95%).

WORKUP

后处理

  1. custompurged 3× with N2
  2. additionPlatinum (20 mg, 20% wt. on activated carbon) was added quickly
  3. custompurged 3× with N2
  4. custompurge cycles with H2
  5. customUpon completion, the reaction vessel was purged of H2
  6. filtrationfiltered over celite
  7. washThe celite was washed several times with methanol until the filtrates
  8. concentrationThe combined filtrates were concentrated