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

HRID 6091

반응식

HRID 6091 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:27])[CH2:22][CH2:23][CH2:24][CH2:25][CH3:26]>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:27])[CH2:22][CH2:23][CH2:24][CH2:25][CH3:26]

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 67340Hexanoyl chlorideHCID 190792594-(3-Aminopropylthio)pyridine dihydrochloride

생성물 1

HCID 152952584-[3-(Caproylamino)propylthio]pyridine수율 81.7%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

To a solution of 600 mg (2.49 mmol) of 4-(3-aminopropylthio)pyridine dihydrochloride and 1.39 ml (9.96 mmol) of triethylamine in 25 ml of methylene chloride was added 0.42 ml (2.99 mmol) of hexanoyl 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=1:10) to obtain 542 mg of the desired compound (81.7%, 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=1:10)

출처 및 근거

ORD 기록
ord-efc045dc445b4acca9722be49a0b70c5
출처 데이터셋
uspto-grants-1993_09
특허 번호
US05246948

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