Benzyl mercaptan → 2-Benzylthio-3-iodopyridine

HRID 260630

반응식

HRID 260630 반응식
F[C:2]1[C:7]([I:8])=[CH:6][CH:5]=[CH:4][N:3]=1.[CH2:9]([SH:16])[C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=1.C(=O)([O-])[O-].[K+].[K+]>C(#N)C>[CH2:9]([S:16][C:2]1[C:7]([I:8])=[CH:6][CH:5]=[CH:4][N:3]=1)[C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=1

참가 물질

5

반응물 3

HCID 7509Benzyl mercaptanHCID 11430Potassium CarbonateHCID 70095012-Fluoro-3-iodopyridine

생성물 1

HCID 150368652-Benzylthio-3-iodopyridine

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

A solution of 34.0 g (0.15 mol) of 2- fluoro-3-iodopyridine and 18.6 g (0.15 mol) of benzylmercaptan in 250 ml of acetonitrile is heated under reflux with 22.8 g (0.165 mol) of potassium carbonate for 8 h. The mixture is cooled, the solvent is removed on a rotary evaporator, the residue is taken up in dichloromethane and the organic phase is washed with water. After drying with sodium sulfate, evaporating and distilling the oily residue in vacuo, 37.3 g (76% of theory) of 2-benzylthio-3-iodopyridine of boiling point 150°-153° C. at 0.1 mbar are obtained.

후처리

  1. temperatureThe mixture is cooled
  2. customthe solvent is removed on a rotary evaporator
  3. washthe organic phase is washed with water
  4. dry with materialAfter drying with sodium sulfate
  5. customevaporating
  6. distillationdistilling the oily residue in vacuo, 37.3 g (76% of theory) of 2-benzylthio-3-iodopyridine of boiling point 150°-153° C. at 0.1 mbar
  7. customare obtained

출처 및 근거

ORD 기록
ord-9cc3456955d741838d7dd4eaba0b23a6
출처 데이터셋
uspto-grants-1996_06
특허 번호
US05529976

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