环丙胺 → 4,5-Dichloro-2-cyclopropylaminobenzenesulphonamide

HRID 17835

反应方程式

HRID 17835 反应方程式
[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

参与物

4

反应物 2

HCID 69828环丙胺HCID 675307044,5-Dichloro-2-fluorobenzenesulfonamide

产物 1

HCID 675298334,5-Dichloro-2-cyclopropylaminobenzenesulphonamide

试剂、催化剂与溶剂 1

HCID 312751,4-二氧六环溶剂

反应条件

温度
105 °C

实验过程

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.

后处理

  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

来源与证据

ORD记录
ord-8df3b2af4ad44a3c9cd5221054a83a8f
来源数据集
uspto-grants-2010_06
专利号
US07741320B2

关联笔记

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