HRID1616918

反应详情

EQUATION

反应方程式

HRID 1616918 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a solution of 7-methoxy-3,4,4a,9a-tetrahydro-1H-benzo[4,5]furo[2,3-c]pyridine-2-carboxylic acid tert-butyl ester (500 mg, 2 mmol) in methanol (7 mL, 200 mmol) was added dropwise a solution of iodine monochloride (340 mg, 2.1 mmol) in 5 ml of methanol at RT. The mixture was stirred overnight at RT. After 18 h, the solvent was removed and the crude reaction mixture was treated with 50 mL of acetonitrile, di-tert-butyl dicarbonate (0.5 mL) and 10 mg of DMAP (10 mg). The mixture was stirred overnight at RT. After 18 h, solvent was removed and the crude product was purified by ISCO chromatography (Hexane:EtOAc 70:30) which was obtained as a syrup (321 mg, 45%). MS m/z 454 [M+H]+

WORKUP

后处理

  1. waitAfter 18 h
  2. customthe solvent was removed
  3. customthe crude reaction mixture
  4. stirringThe mixture was stirred overnight at RT
  5. waitAfter 18 h
  6. customsolvent was removed
  7. customthe crude product was purified by ISCO chromatography (Hexane:EtOAc 70:30) which