Water → 1-Benzyl-1H-benzo[d]imidazol-2(3H)-one

HRID 2229423

반응식

HRID 2229423 반응식
[NH2:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[NH:8][CH2:9][C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=1.Cl[C:17](Cl)([O:19]C(=O)OC(Cl)(Cl)Cl)Cl.O>ClCCl>[CH:13]1[CH:12]=[CH:11][C:10]([CH2:9][N:8]2[C:17](=[O:19])[NH:1][C:2]3[C:3]2=[CH:4][CH:5]=[CH:6][CH:7]=3)=[CH:15][CH:14]=1

참가 물질

5

반응물 3

HCID 962WaterHCID 94429TriphosgeneHCID 2735482N1-Benzylbenzene-1,2-diamine

생성물 1

HCID 7365051-Benzyl-1H-benzo[d]imidazol-2(3H)-one수율 81%

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

[N-(2-Aminophenyl)]-benzylamine (15.1 mmol, 3.0 g) in dichloromethane (80 ml) is charged with triphosgene (5.3 mmol, 1.57 g) in dichloromethane (40 ml) and is stirred at room temperature over the weekend. The suspension is poured into water (100 g) and is extracted with dichloromethane (2×50 ml). The organic layer is a suspension The colorless solid is filtered off, is dried in vacuo and is recrystallized from ethyl acetate to give the title product (81%)(R1=H, R2=benzyl, n=0).

후처리

  1. extractionis extracted with dichloromethane (2×50 ml)
  2. filtrationis filtered off
  3. customis dried in vacuo
  4. customis recrystallized from ethyl acetate

출처 및 근거

ORD 기록
ord-8ced66928dcb40ffa410b7fe06355873
출처 데이터셋
uspto-grants-2002_07
특허 번호
US06420410B1

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