反应 #543580

反应方程式

1-isocyanato-2-methoxybenzene

ethylamine

boron tribromide

→

subtitle compound

N-Ethyl-N′-(2-hydroxyphenyl)urea

溶剂

dichloromethane

dichloromethane

反应条件

后处理

1. 1
   其他Then the volatiles were removed in vacuo
2. 2
   workup.DISSOLUTIONThe residue was redissolved in dichloromethane (15 mL)
3. 3
   洗涤washed 3 times with water
4. 4
   其他The product was purified by HPLC (Kromasil column; eluant:acetonitrile+0.1% trifluoroacetic acid (TFA)/water+0.1% TFA)

实验过程

A solution of 1-isocyanato-2-methoxybenzene (0.32 g, 2.15 mmol) and ethylamine (1 mL) in dichloromethane (15 mL) was stirred at room temperature for 2 days. Then the volatiles were removed in vacuo. The residue was redissolved in dichloromethane (15 mL), and boron tribromide (BBr3) (1 M in dichloromethane (CH2Cl2), 6.5 ml, 6.5 mmol) was added dropwise via syringe under nitrogen. After stirring for 1 h the reaction mixture was diluted with dichloromethane and washed 3 times with water. The product was purified by HPLC (Kromasil column; eluant:acetonitrile+0.1% trifluoroacetic acid (TFA)/water+0.1% TFA) to give subtitle compound (167 mg).

来源