Hydrochloric Acid → 3-(3-Hexylthio-1,2,5-thiadiazol-4-yl)-6-methylpyridine

HRID 965122노트

반응식

HRID 965122 반응식
O.[SH2:2].[Na].Cl[C:5]1[C:9]([C:10]2[CH:11]=[N:12][C:13]([CH3:16])=[CH:14][CH:15]=2)=[N:8][S:7][N:6]=1.C(=O)([O-])[O-].[K+].[K+].[CH2:23](Br)[CH2:24][CH2:25][CH2:26][CH2:27][CH3:28].Cl>CN(C=O)C>[CH2:23]([S:2][C:5]1[C:9]([C:10]2[CH:11]=[N:12][C:13]([CH3:16])=[CH:14][CH:15]=2)=[N:8][S:7][N:6]=1)[CH2:24][CH2:25][CH2:26][CH2:27][CH3:28]

참가 물질

7

반응물 5

HCID 313Hydrochloric AcidHCID 81011-BromohexaneHCID 11430Potassium CarbonateHCID 190752683-(3-Chloro-1,2,5-thiadiazol-4-yl)-6-methylpyridineHCID 53442613Sodium hydrogen sulfide hydrate

생성물 1

HCID 190753693-(3-Hexylthio-1,2,5-thiadiazol-4-yl)-6-methylpyridine

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

Sodium hydrogen sulfide monohydrate (0.33 g, 4.4 mmol) was added to a solution of 3-(3-chloro-1,2,5-thiadiazol-4-yl)-6-methylpyridine (0.85 g, 4 mmol) in DMF (20 ml) at room temperature and the reaction mixture was stirred for 1 h. Potassium carbonate (1.65 g, 12 mmol) and 1-hexylbromide (0.99 g, 6 mmol) were added and the reaction mixture was stirred for additionally 24 h. 1N HCl was added and the reaction mixture was extracted once with ether. The aqueous phase was basified with 50% NaOH and extracted with ether. The ether phases were dried and evaporated to give crude title compound.

후처리

  1. stirringthe reaction mixture was stirred for additionally 24 h
  2. extractionthe reaction mixture was extracted once with ether
  3. extractionextracted with ether
  4. dry with materialThe ether phases were dried
  5. customevaporated

출처 및 근거

ORD 기록
ord-752882fe15e84a0c92bc2f7cc242f1fa
출처 데이터셋
uspto-grants-1998_06
특허 번호
US05773452

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