1H-Imidazole-4-sulfonamide, 5-chloro-1-methyl-N-(3-(4-morpholinyl)propyl)-, monohydrochloride → 1H-Imidazole-4-sulfonamide, 1-methyl-N-(3-(4-morpholinyl)propyl)-

HRID 1708161

반응식

HRID 1708161 반응식
Cl.Cl[C:3]1[N:7]([CH3:8])[CH:6]=[N:5][C:4]=1[S:9]([NH:12][CH2:13][CH2:14][CH2:15][N:16]1[CH2:21][CH2:20][O:19][CH2:18][CH2:17]1)(=[O:11])=[O:10]>[Pd].O>[O:19]1[CH2:18][CH2:17][N:16]([CH2:15][CH2:14][CH2:13][NH:12][S:9]([C:4]2[N:5]=[CH:6][N:7]([CH3:8])[CH:3]=2)(=[O:11])=[O:10])[CH2:21][CH2:20]1

참가 물질

4

반응물 1

HCID 30714611H-Imidazole-4-sulfonamide, 5-chloro-1-methyl-N-(3-(4-morpholinyl)propyl)-, monohydrochloride

생성물 1

HCID 30714701H-Imidazole-4-sulfonamide, 1-methyl-N-(3-(4-morpholinyl)propyl)-

시약·촉매·용매 2

HCID 23938Palladium촉매HCID 962Water용매

실험 절차

16.7 g (46.5 mmol) of 5-chloro-N-(3-morpholino-1-propyl)-1-methyl-4-imidazolesulfonamide hydrochloride from Example 32 are hydrogenated at 25° C. and 3.45 bar in the presence of 3 g of Pd/C catalyst in 250 ml of water. The residue remaining after filtration and evaporation in vacuo is converted into the free base using saturated potassium carbonate solution, extracted with dichloromethane and recrystallized from dioxane/diisopropyl ether in order to give the crystalline title compound, identical with that as in Example 7.

후처리

  1. customare hydrogenated at 25° C.
  2. filtrationafter filtration and evaporation in vacuo
  3. extractionextracted with dichloromethane
  4. customrecrystallized from dioxane/diisopropyl ether in order

출처 및 근거

ORD 기록
ord-2dbbd33826244a74a46908a270ad0a05
출처 데이터셋
uspto-grants-1994_10
특허 번호
US05356922

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