Triethylamine → 2-[3-(Thenoylamino)propylthio]pyridine

HRID 6117

반응식

HRID 6117 반응식
Cl.Cl.[NH2:3][CH2:4][CH2:5][CH2:6][S:7][C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][N:9]=1.C(N(CC)CC)C.[C:21]1([C:26](Cl)=[O:27])[S:25][CH:24]=[CH:23][CH:22]=1>C(Cl)Cl>[C:21]1([C:26]([NH:3][CH2:4][CH2:5][CH2:6][S:7][C:8]2[CH:13]=[CH:12][CH:11]=[CH:10][N:9]=2)=[O:27])[S:25][CH:24]=[CH:23][CH:22]=1

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 789282-Thiophenecarbonyl chlorideHCID 140653253-(Pyridin-2-ylsulfanyl)propan-1-amine dihydrochloride

생성물 1

HCID 190792402-[3-(Thenoylamino)propylthio]pyridine수율 85.5%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

To a solution of 1.50 g (6.22 mmol) of 2-(3-aminopropylthio)pyridine dihydrochloride and 3.19 ml (22.9 mmol) of triethylamine in 60 ml of methylene chloride, 1.09 ml (7.46 mmol) of.2-thenoyl-chloride was added under ice-cooling with stirring. The mixture was stirred at room temperature for 30 minutes. The reaction mixture was washed with a saturated aqueous solution of sodium bicarbonate and water and dried, and then the solvent was distilled off. The residue was purified by column chromatography (eluent: ethyl acetate) to obtain powder. The powder was washed with ether and dried to obtain 1.48 g of the desired compound (yield: 85.5%, colorless powder).

후처리

  1. temperaturecooling
  2. stirringThe mixture was stirred at room temperature for 30 minutes
  3. washThe reaction mixture was washed with a saturated aqueous solution of sodium bicarbonate and water
  4. customdried
  5. distillationthe solvent was distilled off
  6. customThe residue was purified by column chromatography (eluent: ethyl acetate)
  7. customto obtain powder
  8. washThe powder was washed with ether
  9. customdried

출처 및 근거

ORD 기록
ord-9aeedcdb9c5a4914ae3d792adb965e42
출처 데이터셋
uspto-grants-1993_09
특허 번호
US05246948

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