反应 #67429

反应方程式

1-benzo[1,3]dioxol-5-yl-cyclopropanecarbonyl chloride

3-bromo-4-methoxybenzenamine

Et3N

→

1-(benzo[d][1,3]dioxol-5-yl)-N-(3-bromo-4-methoxyphenyl)cyclopropane-carboxamide

溶剂

CH2Cl2

CH2Cl2

CH2Cl2

反应条件

后处理

1. 1
   洗涤The solution was washed with 1N HCl (2×250 mL), sat. aq. NaHCO3 (2×250 mL)
2. 2
   干燥The organics were dried over Na2SO4
3. 3
   过滤filtered
4. 4
   浓缩concentrated in vacuo

实验过程

To a solution of the crude 1-benzo[1,3]dioxol-5-yl-cyclopropanecarbonyl chloride (3.0 mmol) in CH2Cl2 (30 mL) at ambient temperature was added a solution of 3-bromo-4-methoxybenzenamine (3.3 mmol), Et3N (15 mmol), and CH2Cl2 (90 mL) dropwise. The mixture was allowed to stir for 16 h before it was diluted with CH2Cl2 (500 mL). The solution was washed with 1N HCl (2×250 mL), sat. aq. NaHCO3 (2×250 mL), then brine (250 mL). The organics were dried over Na2SO4, filtered, and concentrated in vacuo to provide 1-(benzo[d][1,3]dioxol-5-yl)-N-(3-bromo-4-methoxyphenyl)cyclopropane-carboxamide (B-10) with suitable purity to be used without further purification.

来源