Cyclopropylamine → 4,5-Dichloro-2-cyclopropylaminobenzenesulphonamide

HRID 17835

반응식

HRID 17835 반응식
[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

참가 물질

4

반응물 2

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

생성물 1

HCID 675298334,5-Dichloro-2-cyclopropylaminobenzenesulphonamide

시약·촉매·용매 1

HCID 312751,4-Dioxane용매

반응 조건

온도
105 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-8df3b2af4ad44a3c9cd5221054a83a8f
출처 데이터셋
uspto-grants-2010_06
특허 번호
US07741320B2

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