HRID1014251

反应详情

EQUATION

反应方程式

HRID 1014251 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To the solution of conc. HCl (20 mL) in methanol (40 mL) was added 1-acetyl-5-(methyloxy)-6-nitro-2,3-dihydro-1H-indole (7.8 g, 33 mmol) and the resulting mixture was refluxed for 4 hours. After cooling, the solvent was removed in vacuo, the residue was neutralized with saturated aqueous sodium hydrogencarbonate solution, and a brown precipitate formed. The precipitate was filtered via Buchner funnel, washed with water, and dried under reduced pressure to give 5-(methyloxy)-6-nitro-2,3-dihydro-1H-indole as a brown solid (6.1 g, 94% yield). 1H-NMR (DMSO, 300 MHz) δ 7.11 (s, 1H), 6.87 (s, 1H), 5.59 (brs, 1H), 3.78 (s, 3H), 3.43 (t, 2H), 2.97 (t, 2H).

WORKUP

后处理

  1. temperaturethe resulting mixture was refluxed for 4 hours
  2. temperatureAfter cooling
  3. customthe solvent was removed in vacuo
  4. customa brown precipitate formed
  5. filtrationThe precipitate was filtered via Buchner funnel
  6. washwashed with water
  7. customdried under reduced pressure