4-Chlorophenyl Isocyanate → N-(4-chlorophenyl)-N'-cyclohexanesulfonylurea

HRID 1586852

反応式

HRID 1586852 の反応式
[CH:1]1([S:7]([NH2:10])(=[O:9])=[O:8])[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1.[OH-].[Na+].[Cl:13][C:14]1[CH:19]=[CH:18][C:17]([N:20]=[C:21]=[O:22])=[CH:16][CH:15]=1>CC(C)=O>[Cl:13][C:14]1[CH:19]=[CH:18][C:17]([NH:20][C:21]([NH:10][S:7]([CH:1]2[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]2)(=[O:9])=[O:8])=[O:22])=[CH:16][CH:15]=1

参加物

5

反応物 3

HCID 76934-Chlorophenyl IsocyanateHCID 14798Sodium HydroxideHCID 75536Cyclohexanesulfonamide

生成物 1

HCID 22131300N-(4-chlorophenyl)-N'-cyclohexanesulfonylurea収率 70.1%

試薬・触媒・溶媒 1

HCID 180Acetone溶媒2 回

実験手順

The general method of procedure A was followed with cyclohexanesulfonamide (1.89 g), acetone (5 ml), 1N sodium hydroxide (11.6 ml). After stirring overnight at room temperature, the mixture was cooled in an ice bath and 4-chlorophenyl isocyanate (1.89 g) dissolved in acetone (5 ml) was added. The mixture was warmed to room temperature and stirred two days, filtered, and the separated white solid washed with water. The filtrates were combined and treated with glacial acetic acid (1 ml) followed by addition of water. The resulting solid was collected by filtration, washed with water and air dried to provide 2.57 g of a tan powder.

後処理

  1. temperaturethe mixture was cooled in an ice bath
  2. additionwas added
  3. temperatureThe mixture was warmed to room temperature
  4. stirringstirred two days
  5. filtrationfiltered
  6. washthe separated white solid washed with water
  7. additiontreated with glacial acetic acid (1 ml)
  8. additionfollowed by addition of water
  9. filtrationThe resulting solid was collected by filtration
  10. washwashed with water and air
  11. customdried

出典と根拠

ORDレコード
ord-5bb114658b344e489df75f7d16931279
出典データセット
uspto-grants-1993_06
特許番号
US05216026

関連ノート

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