Hydrochloric Acid → 1-Butanesulfonamide, 2-ethyl-2-(((1,2,4)triazolo(1,5-b)pyridazin-6-yloxy)methyl)-

HRID 274266

반응식

HRID 274266 반응식
[H-].[Na+].[OH:3][CH2:4][C:5]([CH2:13][CH3:14])([CH2:11][CH3:12])[CH2:6][S:7]([NH2:10])(=[O:9])=[O:8].Cl[C:16]1[CH:17]=[CH:18][C:19]2[N:20]([N:22]=[CH:23][N:24]=2)[N:21]=1.Cl>CN(C)C=O.O>[CH2:11]([C:5]([CH2:13][CH3:14])([CH2:6][S:7](=[O:8])(=[O:9])[NH2:10])[CH2:4][O:3][C:16]1[CH:17]=[CH:18][C:19]2[N:20]([N:22]=[CH:23][N:24]=2)[N:21]=1)[CH3:12]

참가 물질

7

반응물 4

HCID 313Hydrochloric AcidHCID 24758Sodium hydrideHCID 105597653-Hydroxy-2,2-diethyl-1-propanesulfonamideHCID 112406116-Chloro-(1,2,4)triazolo(1,5-b)pyridazine

생성물 1

HCID 30737831-Butanesulfonamide, 2-ethyl-2-(((1,2,4)triazolo(1,5-b)pyridazin-6-yloxy)methyl)-수율 62.7%

시약·촉매·용매 2

HCID 962Water용매HCID 6228Dimethylformamide용매

실험 절차

In 20 ml of dimethylformamide was suspended 0.64 g of 60% sodium hydride in oil, followed by addition of 1.56 g of 3-hydroxy-2,2-diethyl-1-propanesulfonamide and the mixture was stirred under reduced pressure at room temperatue for 30 minutes. Then, 1.24 g of 6-chloro[1,2,4]triazolo[1,5-b]pyridazine was added and the mixture was further stirred at room temperature for 1.5 hours. Following addition of 100 ml of iced water, the reaction mixture was adjusted to pH 6 with 1N-hydrochloric acid and the resulting crystals were collected by filtration and washed with 20 ml of water and 20 ml of ethyl ether. The washed crystals were recrystallized from hot ethanol to provide 1.57 g of the title compound. m.p. 194°-197° C.

후처리

  1. stirringthe mixture was further stirred at room temperature for 1.5 hours
  2. filtrationthe resulting crystals were collected by filtration
  3. washwashed with 20 ml of water and 20 ml of ethyl ether
  4. customThe washed crystals were recrystallized from hot ethanol

출처 및 근거

ORD 기록
ord-e0e8c60a03fc460dba29e649e2ab0274
출처 데이터셋
uspto-grants-1995_02
특허 번호
US05389633

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