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

HRID 2229423ノート

反応式

HRID 2229423 の反応式
[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

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

[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).

後処理

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

出典と根拠

ORDレコード
ord-8ced66928dcb40ffa410b7fe06355873
出典データセット
uspto-grants-2002_07
特許番号
US06420410B1

反応ノート

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