Ammonia → HCID 178425298、化合物

HRID 1091027ノート

反応式

HRID 1091027 の反応式
[NH2:1][C:2]([C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][C:5]=1[NH:10][C:11](=S)[NH:12][C:13](=[O:21])[C:14]1[CH:19]=[CH:18][CH:17]=[C:16]([CH3:20])[CH:15]=1)=[O:3].N>OO>[O:3]=[C:2]1[C:4]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)[NH:10][C:11]([NH:12][C:13](=[O:21])[C:14]2[CH:19]=[CH:18][CH:17]=[C:16]([CH3:20])[CH:15]=2)=[N:1]1

参加物

4

反応物 2

HCID 222AmmoniaHCID 667545N-[(2-carbamoylphenyl)carbamothioyl]-3-methylbenzamide

生成物 1

HCID 178425298HCID 178425298、化合物収率 27.7%

試薬・触媒・溶媒 1

HCID 784Hydrogen Peroxide溶媒2 回

実験手順

To a stirred mixture of 9.3 g of the above benzamide and 200 ml of methanolic ammonia was added dropwise, 10 ml of 30% hydrogen peroxide over 3 minutes. An exotherm required cooling in an ice bath. A 15 ml portion of 30% hydrogen peroxide was added, the mixture was stirred 48 hours, the solid collected, and mixed with 100 ml of hot water. This solid was collected, mixed with 400 ml of hot acetonitrile and filtered. The filtrate was chilled, giving 2.3 g of the desired product as off-white crystals, mp 211°-213° C.

後処理

  1. additionwas added dropwise
  2. temperatureAn exotherm required cooling in an ice bath
  3. customthe solid collected
  4. additionmixed with 100 ml of hot water
  5. customThis solid was collected
  6. additionmixed with 400 ml of hot acetonitrile
  7. filtrationfiltered
  8. temperatureThe filtrate was chilled

出典と根拠

ORDレコード
ord-8dc2e2cda81048fc8de8477320eae473
出典データセット
uspto-grants-1992_01
特許番号
US05084457

反応ノート

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