反応 #543541

反応方程式

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

isoamyl nitrite

hydrochloric acid

→

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

反応条件

後処理

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
   その他The solid formed
4. 4
   ろ過was filtered
5. 5
   洗浄washed with cold ether:ethanol (3:1, 150 mL)
6. 6
   その他dried
7. 7
   その他It was crystallized from acetonitrile

実験手順

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.

出典