Acetic Acid → N-(2-cycloheptenyl)dichloromaleinimide

HRID 247620

반응식

HRID 247620 반응식
[CH:1]1([NH2:8])[CH2:7][CH2:6][CH2:5][CH2:4][CH:3]=[CH:2]1.[Cl:9][C:10]1=[C:11]([Cl:17])[C:12]([O:14][C:15]1=O)=[O:13].C(O)(=O)C>CCOCC>[CH:1]1([N:8]2[C:15](=[O:14])[C:10]([Cl:9])=[C:11]([Cl:17])[C:12]2=[O:13])[CH2:7][CH2:6][CH2:5][CH2:4][CH:3]=[CH:2]1

참가 물질

5

반응물 3

HCID 176Acetic AcidHCID 70728Dichloromaleic anhydrideHCID 11263481Cyclohept-2-en-1-amine

생성물 1

HCID 13578660N-(2-cycloheptenyl)dichloromaleinimide수율 70.7%

시약·촉매·용매 1

HCID 3283Diethyl Ether용매

실험 절차

A mixture of 2-cycloheptenylamine (1.01 g), dichloromaleic anhydride (1.67 g) and acetic acid (10 ml) was heated under reflux for 3 hours. After cooling, ether (20 ml) was added to the reaction mixture which was then washed with a saturated aqueous sodium hydrogencarbonate solution, water and a saturated aqueous sodium chloride solution in this order. The organic layer was dried over anhydrous magnesium sulfate and concentrated. The deposited crystal was purified by recrystallization from hexane to obtain 1.67 g of N-(2-cycloheptenyl)dichloromaleinimide [Compound (217)].

후처리

  1. temperaturewas heated
  2. temperatureunder reflux for 3 hours
  3. temperatureAfter cooling
  4. washwas then washed with a saturated aqueous sodium hydrogencarbonate solution, water
  5. dry with materialThe organic layer was dried over anhydrous magnesium sulfate
  6. concentrationconcentrated
  7. customThe deposited crystal was purified by recrystallization from hexane

출처 및 근거

ORD 기록
ord-abdfc592559a4f5aa99b7d586c93a409
출처 데이터셋
uspto-grants-1987_11
특허 번호
US04709052

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