Hydrochloric Acid → 2-Ethylthio-6-n-propylimidazo[1,2-b]pyridazin-3-ylsulfonamide

HRID 1946444노트

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HRID 1946444 반응식
[H-].[Na+].[CH2:3]([SH:5])[CH3:4].Cl[C:7]1[N:8]=[C:9]2[CH:14]=[CH:13][C:12]([CH2:15][CH2:16][CH3:17])=[N:11][N:10]2[C:18]=1[S:19]([NH2:22])(=[O:21])=[O:20].Cl>CN(C=O)C.O>[CH2:3]([S:5][C:7]1[N:8]=[C:9]2[CH:14]=[CH:13][C:12]([CH2:15][CH2:16][CH3:17])=[N:11][N:10]2[C:18]=1[S:19]([NH2:22])(=[O:21])=[O:20])[CH3:4]

참가 물질

7

반응물 4

HCID 313Hydrochloric AcidHCID 6343EthanethiolHCID 24758Sodium hydrideHCID 230281102-Chloro-6-propylimidazo[1,2-b]pyridazine-3-sulfonamide

생성물 1

HCID 230281222-Ethylthio-6-n-propylimidazo[1,2-b]pyridazin-3-ylsulfonamide

시약·촉매·용매 2

HCID 962Water용매HCID 6228Dimethylformamide용매

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온도
0 °C

실험 절차

Sodium hydride (60%, 0.73 g, 18.2 mmol) was suspended in DMF (10.0 ml) under ice-cooling, and ethanethiol (1.35 ml, 18.2 mmol) was added dropwise thereto, and the mixture was stirred at 0° C. for 2 hours. 2-Chloro-6-propylimidazo[1,2-b]pyridazin-3-ylsulfonamide (1.00 g, 3.64 mmol) was added thereto and heated at 110° C. for 2.5 hours under stirring. The reaction mixture was left, cooled, diluted with water and acidified by dropwise addition of conc. hydrochloric acid. The precipitated solids were collected by filtration and washed with water, and the solids were suspended in a mixed solvent of chloroform and ethyl acetate, and the insoluble solids were collected by filtration, and the solids were washed with chloroform to give the title compound as gray crystals. The yield was 0.45 g (41.2%).

후처리

  1. temperaturecooling
  2. temperatureheated at 110° C. for 2.5 hours
  3. stirringunder stirring
  4. waitThe reaction mixture was left
  5. temperaturecooled
  6. filtrationThe precipitated solids were collected by filtration
  7. washwashed with water
  8. filtrationthe insoluble solids were collected by filtration
  9. washthe solids were washed with chloroform

출처 및 근거

ORD 기록
ord-a9e5bfeac39f43c9a212871060b6171c
출처 데이터셋
uspto-grants-2013_03
특허 번호
US08399381B2

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