HRID2174939

反应详情

EQUATION

反应方程式

HRID 2174939 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

6-Bromo-4-chloro-3-nitroquinoline (compound of step 1, 5.2 mmol) and 6-methoxypyridin-3-amine (commercially available, 5.2 mmol) was dissolved in acetic acid (5 mL) and the mixture was stirred overnight. Water was added and the yellow precipitate was filtered off. The precipitate was washed with water and dried. The solid obtained was partitioned and extracted with EtOAc and THF, washed with saturated aqueous NaHCO3. The organic layer was dried over anhydrous sodium sulfate and concentrated to obtain the title compound. 1H NMR (DMSO-d6, 300 MHz): 10.03 (s, 1H), 9.01 (s, 1H), 8.72 (d, J=1.5 Hz, 1H), 8.04-7.90 (m, 3H), 7.50 (dd, J=2.4, 8.7 Hz, 1H), 6.82 (d, J=9.0 Hz, 1H), 3.85 (s, 3H); MS (m/z): 377.0 (M+1)+.

WORKUP

后处理

  1. filtrationthe yellow precipitate was filtered off
  2. washThe precipitate was washed with water
  3. customdried
  4. customThe solid obtained
  5. customwas partitioned
  6. extractionextracted with EtOAc and THF
  7. washwashed with saturated aqueous NaHCO3
  8. dry with materialThe organic layer was dried over anhydrous sodium sulfate
  9. concentrationconcentrated