HRID480575

反应详情

EQUATION

反应方程式

HRID 480575 的结构方程式

PROCEDURE

实验过程

To a 1 L round-bottomed flask equipped with a magnetic stirrer and a N2 bubbler were added 2-methyl-3-trichloroacetyl-7-methoxyindole (22.8 g, 74.37 mmol) and MeOH (150 mL). The mixture was stirred at RT to give a slurry. KOH (42.5 wt %, 2 mL) was added and the reaction stirred for 5 min. HCl (0.1N, 500 mL) was added dropwise. The slurry was stirred at RT for 1 h and filtered. The cake was washed with DI water (3×30 mL) and suction dried for 18 h to give 2-methyl-3-methoxycarbonyl-7-methoxyindole (15.57 g, 96% yield). 1H NMR (CDCl3) δ2.71 (s, 3H), 3.89 (s, 3H), 3.92 (s, 3H), 6.63 (d, J=7.9 Hz, 1H), 7.12 (dd, J=7.9, 8.0 Hz, 1H), 7.66 (d, J=8.0 Hz, 1H), 8.84 (s, 1H).

WORKUP

后处理

  1. customTo a 1 L round-bottomed flask equipped with a magnetic stirrer
  2. customto give a slurry
  3. stirringthe reaction stirred for 5 min
  4. stirringThe slurry was stirred at RT for 1 h
  5. filtrationfiltered
  6. washThe cake was washed with DI water (3×30 mL) and suction
  7. customdried for 18 h