反应 #543541

反应方程式

4-methyl-1-(phthalimido)-3-pentene

isoamyl nitrite

hydrochloric acid

→

4-Chloro-4-methyl-1-(phthalimido)-3-nitrosopentane

反应条件

后处理

1. 1
   温度The reaction mixture was maintained below 5° C. during the addition
2. 2
   workup.STIRRINGstirred at 5° C. for an additional 2 h
3. 3
   其他The solid formed
4. 4
   过滤was filtered
5. 5
   洗涤washed with cold ether:ethanol (3:1, 150 mL)
6. 6
   其他dried
7. 7
   其他It was crystallized from acetonitrile

实验过程

To a cooled (0-5° C.) solution of 4-methyl-1-(phthalimido)-3-pentene (5.0 g, 0.022 mol) and isoamyl nitrite (13.0 g, 15 mL, 0.11 mol) was added concentrated hydrochloric acid (4.0 mL, 0.04 mol) with stirring. The reaction mixture was maintained below 5° C. during the addition and stirred at 5° C. for an additional 2 h. The solid formed was filtered and washed with cold ether:ethanol (3:1, 150 mL) and dried. Yield: 4.72 g (72.8%). It was crystallized from acetonitrile. mp 140-141° C. MS: (M+H)+=296.0.

来源