Cyclopropylamine → 4,5-Dichloro-2-cyclopropylaminobenzenesulphonamide

HRID 17835

反応式

HRID 17835 の反応式
[Cl:1][C:2]1[C:7]([Cl:8])=[CH:6][C:5]([S:9]([NH2:12])(=[O:11])=[O:10])=[C:4](F)[CH:3]=1.[CH:14]1([NH2:17])[CH2:16][CH2:15]1>O1CCOCC1>[Cl:1][C:2]1[C:7]([Cl:8])=[CH:6][C:5]([S:9]([NH2:12])(=[O:11])=[O:10])=[C:4]([NH:17][CH:14]2[CH2:16][CH2:15]2)[CH:3]=1

参加物

4

反応物 2

HCID 69828CyclopropylamineHCID 675307044,5-Dichloro-2-fluorobenzenesulfonamide

生成物 1

HCID 675298334,5-Dichloro-2-cyclopropylaminobenzenesulphonamide

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒

反応条件

温度
105 °C

実験手順

A solution of 4,5-dichloro-2-fluorobenzenesulphonamide (3 g) in dioxane (30 mL) to which cyclopropylamine (3 mL) has been added is heated at 100-110° C. in a hermetically closed vessel for 24 hours. The solvent and the excess of amine are removed by distillation under reduced pressure and the residue is dissolved in methanol (20 mL). The methanolic solution is cooled on an ice bath, and water (60 mL) is added. The precipitate obtained (the title product) is collected by filtration, washed with water and dried. It is used in the following Step without being otherwise purified.

後処理

  1. customThe solvent and the excess of amine are removed by distillation under reduced pressure
  2. dissolutionthe residue is dissolved in methanol (20 mL)
  3. temperatureThe methanolic solution is cooled on an ice bath
  4. additionwater (60 mL) is added

出典と根拠

ORDレコード
ord-8df3b2af4ad44a3c9cd5221054a83a8f
出典データセット
uspto-grants-2010_06
特許番号
US07741320B2

関連ノート

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