HRID506783

反应详情

EQUATION

反应方程式

HRID 506783 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Reflux bisazaindole 29 (40 mg, 0.081 mmol) in KOH at 4%/MeOH (10 mL) for 5.5 h and then concentrate the reaction under vacuum. Purification on SiO2 (MeOH at 2-4%/CH2Cl2) leads to 30 (13 mg, 47.3%) as a white solid: 1H NMR (CDCl3) δ 10.92 (s broad, 1H), 8.07 (d, 1H, J=5.3 Hz), 7.49 (s, 1H), 7.05 (s apparent overlapping d, 2H, J=5.2 Hz), 6.62 (s, 1H), 4.22 (s, 3H), 3.96 (s, 3H), 3.81 (s, 3H), TLC (EtOAc at 40%/heptane), Rf=0.40, m/z obs.=343.3 (M+1), 345.3.

WORKUP

后处理

  1. concentrationconcentrate
  2. customthe reaction under vacuum
  3. customPurification on SiO2 (MeOH at 2-4%/CH2Cl2)