Acetic Acid → N-(2-cycloheptenyl)dichloromaleinimide

HRID 247620

反応式

HRID 247620 の反応式
[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

参加物

5

反応物 3

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

生成物 1

HCID 13578660N-(2-cycloheptenyl)dichloromaleinimide収率 70.7%

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒

実験手順

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)].

後処理

  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

出典と根拠

ORDレコード
ord-abdfc592559a4f5aa99b7d586c93a409
出典データセット
uspto-grants-1987_11
特許番号
US04709052

関連ノート

読み込み中…