HRID1895164

反应详情

EQUATION

反应方程式

HRID 1895164 的结构方程式

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

A mixture of methyl 2-[(3-bromo-2-fluorophenyl)hydrazono]-4-methoxy-3-oxobutanoate (5.36 g, 15.4 mmol) in N,N-dimethylformamide dimethyl acetal (54 mL) was heated to reflux for 2 h and cooled to 0° C. The precipitates were collected by filtration, washed with hexane and dried to yield the title compound (4.16 g, 75% yield) as a brown solid: 1H NMR (DMSO-d6, 300 MHz): δ ppm 3.80 (3H, s), 3.83 (3H, s), 7.40 (1H, td, J=8.1, 1.1 Hz), 7.75-7.84 (1H, m), 7.94 (1H, ddd, J=8.1, 6.4, 1.7 Hz), 8.60 (1H, d, J=1.9 Hz).

WORKUP

后处理

  1. temperaturewas heated
  2. temperatureto reflux for 2 h
  3. filtrationThe precipitates were collected by filtration
  4. washwashed with hexane
  5. customdried