Triethylamine → 4-[3-(Butyrylamino)propylthio]pyridine

HRID 6090

반응식

HRID 6090 반응식
Cl.Cl.[NH2:3][CH2:4][CH2:5][CH2:6][S:7][C:8]1[CH:13]=[CH:12][N:11]=[CH:10][CH:9]=1.C(N(CC)CC)C.[C:21](Cl)(=[O:25])[CH2:22][CH2:23][CH3:24]>C(Cl)Cl>[C:21]([NH:3][CH2:4][CH2:5][CH2:6][S:7][C:8]1[CH:13]=[CH:12][N:11]=[CH:10][CH:9]=1)(=[O:25])[CH2:22][CH2:23][CH3:24]

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 8855Butyryl chlorideHCID 190792594-(3-Aminopropylthio)pyridine dihydrochloride

생성물 1

HCID 152952574-[3-(Butyrylamino)propylthio]pyridine수율 91.1%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

To a solution of 700 mg (2.90 mmol) of 4-(3-aminopropylthio)pyridine dihydrochloride and 1.62 ml (11.6 mmol) of triethylamine in 30 ml of methylene chloride was added 0.36 ml (3.48 mmol) of butyryl chloride under ice-cooling with stirring and the mixture was stirred at room temperature for 30 minutes. The reaction mixture was washed with an aqueous saturated sodium bicarbonate solution and water and dried. The solvent was distilled off. The residue was purified by column chromatography (eluent: methanol/ethyl acetate=1:1) to obtain 630 mg of the desired compound (91.1%, pale yellow oil).

후처리

  1. temperaturecooling
  2. stirringthe mixture was stirred at room temperature for 30 minutes
  3. washThe reaction mixture was washed with an aqueous saturated sodium bicarbonate solution and water
  4. customdried
  5. distillationThe solvent was distilled off
  6. customThe residue was purified by column chromatography (eluent: methanol/ethyl acetate=1:1)

출처 및 근거

ORD 기록
ord-4a1694bb3df64335856b4b663a854296
출처 데이터셋
uspto-grants-1993_09
특허 번호
US05246948

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