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

HRID 232693ノート

反応式

HRID 232693 の反応式
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]

参加物

7

反応物 5

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

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 basilled with 50% NaOH and extracted with ether. The ether phases were dried and evaporated to give crude title compound.

後処理

  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

出典と根拠

ORDレコード
ord-bec5e5b8fed74da88e00afc4b8ce1ff3
出典データセット
uspto-grants-1997_01
特許番号
US05591755

反応ノート

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