Triethylamine → 3-(3,3-Diphenyl-ureido)-N-phenylbenzamide

HRID 610080

反応式

HRID 610080 の反応式
[NH2:1][C:2]1[CH:3]=[C:4]([CH:14]=[CH:15][CH:16]=1)[C:5]([NH:7][C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1)=[O:6].[C:17]1([N:23]([C:27]2[CH:32]=[CH:31][CH:30]=[CH:29][CH:28]=2)[C:24](Cl)=[O:25])[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=1.C(N(CC)CC)C>C(O)C>[C:17]1([N:23]([C:27]2[CH:32]=[CH:31][CH:30]=[CH:29][CH:28]=2)[C:24](=[O:25])[NH:1][C:2]2[CH:3]=[C:4]([CH:14]=[CH:15][CH:16]=2)[C:5]([NH:7][C:8]2[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=2)=[O:6])[CH:18]=[CH:19][CH:20]=[CH:21][CH:22]=1

参加物

5

反応物 3

HCID 8471TriethylamineHCID 65741N,N-Diphenylcarbamic chlorideHCID 843473-Aminobenzanilide

生成物 1

HCID 196009793-(3,3-Diphenyl-ureido)-N-phenylbenzamide収率 42.6%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

A mixture of 3-amino-N-phenylbenzamide (2.0 g, 9.4 mmol), diphenylcarbamoyl chloride (2.2 g, 9.4 mmol) and triethylamine (2.6 mL, 19 mmol) in ethanol (10 mL) was heated to reflux for 4.5 hours. The mixture was cooled and concentrated, water was added, the slurry was acidified with 1 N HCl and the solid was collected, washed with water, dried and recrystallized from acetone/hexanes, to give a colorless solid (1.63 g, 42%).

後処理

  1. temperaturewas heated
  2. temperatureto reflux for 4.5 hours
  3. temperatureThe mixture was cooled
  4. concentrationconcentrated
  5. additionwater was added
  6. customthe solid was collected
  7. washwashed with water
  8. customdried
  9. customrecrystallized from acetone/hexanes

出典と根拠

ORDレコード
ord-b4ea39b9f4e54985812f70768033485a
出典データセット
uspto-grants-1999_12
特許番号
US05998463

関連ノート

読み込み中…