Thiophenol → 2-[(Phenylsulfanyl)methyl]pyridine--hydrogen chloride (1/1)

HRID 1649131노트

반응식

HRID 1649131 반응식
[C:1]1([SH:7])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[Na].Cl.[N:10]1[CH:15]=[CH:14][CH:13]=[CH:12][C:11]=1[CH2:16][Cl:17]>C(O)C>[ClH:17].[C:1]1([S:7][CH2:16][C:11]2[CH:12]=[CH:13][CH:14]=[CH:15][N:10]=2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1

참가 물질

5

반응물 3

HCID 7969ThiophenolHCID 23392Picolyl chloride hydrochlorideHCID 5360545Sodium

생성물 1

HCID 124744352-[(Phenylsulfanyl)methyl]pyridine--hydrogen chloride (1/1)수율 5.9%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

Thiophenol (21 ml) was added to a solution of sodium (4.6 g) in ethanol (100 ml). To the resulting solution was added 2-picolyl chloride, hydrochloride (15 g) and the mixture was heated at reflux for 2 hours. Precipitated sodium chloride was removed by filtration and the solution was acidified with ethereal HCl. The solvent was removed by evaporation and the residue induced to crystallise by trituration with ether. Recrystallisation from ethanol-ether gave 2-((phenylthio)-methyl)pyridine, hydrochloride (5.0 g) mp 142°-4° C. (Found: C,60.6; H,5.25; N,5.5, C12H11NS,HCl requires C,60.6: H,5.1: N,5.9%).

후처리

  1. temperaturethe mixture was heated
  2. temperatureat reflux for 2 hours
  3. customPrecipitated sodium chloride was removed by filtration
  4. customThe solvent was removed by evaporation
  5. customthe residue induced to crystallise by trituration with ether
  6. customRecrystallisation from ethanol-ether

출처 및 근거

ORD 기록
ord-fe9241d55f4547ce8605df4ae1671be0
출처 데이터셋
uspto-grants-1983_11
특허 번호
US04415579

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