HRID1497265

反应详情

EQUATION

反应方程式

HRID 1497265 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
300 °C

PROCEDURE

实验过程

A solution of (2-amino-4-methoxy-phenyl)-phenyl-methanone (400 mg, 1.76 mmol) and ethyl 2-cyanoacetate (239 mg, 225 μl) in toluene (6 ml) containing catalytic amounts of piperidine (15.0 mg, 17.4 μl) was pumped at a flow rate of 0.42 ml min−1 (residence time 40 min) through a steel reactor coil (volume=17 ml) that was heated to 300° C. The reaction mixture was evaporated to dryness and the remaining solid was triturated with CH2Cl2/heptane 2:1 for 3 h. The solid was filtrated off and washed two times with CH2Cl2/heptane 1:1 to give the title compound (140 mg, 29%) as off-white solid. MS (ESI): 277.4 (M+H)+.

WORKUP

后处理

  1. customwas pumped at a flow rate of 0.42 ml min−1 (residence time 40 min) through a steel reactor
  2. customThe reaction mixture was evaporated to dryness
  3. customthe remaining solid was triturated with CH2Cl2/heptane 2:1 for 3 h
  4. filtrationThe solid was filtrated off
  5. washwashed two times with CH2Cl2/heptane 1:1