تفاعل #543541
ord-db9272fcc54841b88676ea04e0f46721
معادلة التفاعل
4-methyl-1-(phthalimido)-3-pentene
isoamyl nitrite
hydrochloric acid
→
4-Chloro-4-methyl-1-(phthalimido)-3-nitrosopentane
الكواشف
لا شيء
ظروف التفاعل
الظروف التفصيلية
See reaction.notes.procedure_details.
المعالجة
- 1درجة الحرارةThe reaction mixture was maintained below 5° C. during the addition
- 2workup.STIRRINGstirred at 5° C. for an additional 2 h
- 3أخرىThe solid formed
- 4ترشيحwas filtered
- 5غسيلwashed with cold ether:ethanol (3:1, 150 mL)
- 6أخرىdried
- 7أخرىIt was crystallized from acetonitrile
الإجراء التجريبي
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.