HRID1066769

反应详情

EQUATION

反应方程式

HRID 1066769 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

3-Amino-6-methyl-5,6,7,8-tetrahydro[1,6]naphthyridine D4 (900 mg, 5.52 mmol) was dissolved in acetic acid (50 ml) before being treated portionwise with N-chlorosuccinimide (1.11 g, 8.28 mmol) 20 min. The reaction mixture was stirred overnight at room temperature under argon. The reaction mixture was diluted with water (125 ml), basified to pH10 with solid K2CO3 and extracted with dichloromethane (×2). The combined organic extracts were washed with sodium bicarbonate, dried (MgSO4) and evaporation in vacuo gave a crude black solid. Flash chromatography using dichloromethane (10% MeOH) gave thetitle compound as a pale orange solid.

WORKUP

后处理

  1. extractionextracted with dichloromethane (×2)
  2. washThe combined organic extracts were washed with sodium bicarbonate
  3. customdried
  4. custom(MgSO4) and evaporation in vacuo
  5. customgave a crude black solid
  6. customgave thetitle compound as a pale orange solid