반응 #543541

반응 방정식

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

isoamyl nitrite

hydrochloric acid

→

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

반응 조건

후처리

1. 1
   온도The reaction mixture was maintained below 5° C. during the addition
2. 2
   workup.STIRRINGstirred at 5° C. for an additional 2 h
3. 3
   기타The solid formed
4. 4
   여과was filtered
5. 5
   세척washed with cold ether:ethanol (3:1, 150 mL)
6. 6
   기타dried
7. 7
   기타It was crystallized from acetonitrile

실험 절차

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.

출처