4-Chlorophenyl Isocyanate → 1-(N-(4-chlorophenyl)-carbamoyl)-2-(2,3-dimethylanilinomethyl)-2-imidazoline

HRID 903160노트

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HRID 903160 반응식
[CH3:1][C:2]1[C:14]([CH3:15])=[CH:13][CH:12]=[CH:11][C:3]=1[NH:4][CH2:5][C:6]1[NH:7][CH2:8][CH2:9][N:10]=1.[Cl:16][C:17]1[CH:22]=[CH:21][C:20]([N:23]=[C:24]=[O:25])=[CH:19][CH:18]=1>C(Cl)Cl>[Cl:16][C:17]1[CH:22]=[CH:21][C:20]([NH:23][C:24]([N:10]2[CH2:9][CH2:8][N:7]=[C:6]2[CH2:5][NH:4][C:3]2[CH:11]=[CH:12][CH:13]=[C:14]([CH3:15])[C:2]=2[CH3:1])=[O:25])=[CH:19][CH:18]=1

참가 물질

4

반응물 2

HCID 76934-Chlorophenyl IsocyanateHCID 1287552,3-Xylylaminomethyl-2'-imidazoline

생성물 1

HCID 233378931-(N-(4-chlorophenyl)-carbamoyl)-2-(2,3-dimethylanilinomethyl)-2-imidazoline

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

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온도
0 °C

실험 절차

2-(2,3-Dimethylanilinomethyl)-2-imidazoline (4.20 g; 0.024 moles) was stirred in methylene chloride (90 ml), cooled to 0° C. and a solution of 4-chlorophenyl isocyanate (3.66 g; 0.024 moles) in methylene chloride (10 ml) was then added dropwise. A white precipitate formed rapidly. Stirring was continued for 2 to 3 hours after the addition at 0° C., the reaction mixture then allowed to reach ambient temperature and stirring was continued overnight. The reaction mixture was then evaporated to dryness under reduced pressure and the solid residue so obtained recrystallised from propan-2-ol to yield white crystals of 1-(N-(4-chlorophenyl)-carbamoyl)-2-(2,3-dimethylanilinomethyl)-2-imidazoline m.p. 153°-155° C.

후처리

  1. customA white precipitate formed rapidly
  2. additionafter the addition at 0° C.
  3. customto reach ambient temperature
  4. stirringstirring
  5. waitwas continued overnight
  6. customThe reaction mixture was then evaporated to dryness under reduced pressure
  7. customthe solid residue so obtained
  8. customrecrystallised from propan-2-ol

출처 및 근거

ORD 기록
ord-a0b106ecdabb40daa1137581a50e9d68
출처 데이터셋
uspto-grants-1980_10
특허 번호
US04226876

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