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

HRID 274266

反応式

HRID 274266 の反応式
[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]

参加物

7

反応物 4

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

生成物 1

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

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6228Dimethylformamide溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-e0e8c60a03fc460dba29e649e2ab0274
出典データセット
uspto-grants-1995_02
特許番号
US05389633

関連ノート

読み込み中…