Triethylamine → 4-(4-Chlorobutylthio)pyridine

HRID 6190

반응식

HRID 6190 반응식
[SH:1][C:2]1[CH:7]=[CH:6][N:5]=[CH:4][CH:3]=1.Br[CH2:9][CH2:10][CH2:11][CH2:12][Cl:13].C(N(CC)CC)C>C(O)C>[Cl:13][CH2:12][CH2:11][CH2:10][CH2:9][S:1][C:2]1[CH:7]=[CH:6][N:5]=[CH:4][CH:3]=1

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 813641-Bromo-4-chlorobutaneHCID 178418431pyridine-4-thiol

생성물 1

HCID 158169784-(4-Chlorobutylthio)pyridine수율 89.7%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

To a suspension of 33.35 g (0.30 mol) of 4-mercaptopyridine and 51.44 g (0.30 mol) of 1-bromo-4-chlorobutane in 500 ml of ethanol, 41.9 ml (0.30 mol) of triethylamine was added, and the mixture was stirred at room temperature for 5 hours. The solvent was distilled off and chloroform was added to the residue. The mixture was washed with water and dried over anhydrous magnesium sulfate. The solvent was distilled off and the residue was purified by column chromatography (eluent: ethyl acetate/n-hexane =1:1) to give 54.27 g of the desired compound (89.7% yield, colorless oil).

후처리

  1. additionwas added
  2. distillationThe solvent was distilled off
  3. additionchloroform was added to the residue
  4. washThe mixture was washed with water
  5. dry with materialdried over anhydrous magnesium sulfate
  6. distillationThe solvent was distilled off
  7. customthe residue was purified by column chromatography (eluent: ethyl acetate/n-hexane =1:1)

출처 및 근거

ORD 기록
ord-4aaaa3a6821445dabee298f6b50af2bd
출처 데이터셋
uspto-grants-1993_09
특허 번호
US05246948

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