HRID1497265
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
产物
AUXILIARIES
试剂、催化剂与溶剂
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
- customwas pumped at a flow rate of 0.42 ml min−1 (residence time 40 min) through a steel reactor
- customThe reaction mixture was evaporated to dryness
- customthe remaining solid was triturated with CH2Cl2/heptane 2:1 for 3 h
- filtrationThe solid was filtrated off
- washwashed two times with CH2Cl2/heptane 1:1