Water → 2-Chloro-4-(3-methyl-4-methylmercapto-phenoxy)-pyridine

HRID 1262781

반응식

HRID 1262781 반응식
[CH3:1][C:2]1[CH:3]=[C:4]([OH:10])[CH:5]=[CH:6][C:7]=1[S:8][CH3:9].[Cl:11][C:12]1[CH:17]=[C:16]([N+]([O-])=O)[CH:15]=[CH:14][N:13]=1.C([O-])([O-])=O.[K+].[K+].O>C(#N)C>[Cl:11][C:12]1[CH:17]=[C:16]([O:10][C:4]2[CH:5]=[CH:6][C:7]([S:8][CH3:9])=[C:2]([CH3:1])[CH:3]=2)[CH:15]=[CH:14][N:13]=1

참가 물질

6

반응물 4

HCID 962WaterHCID 11430Potassium CarbonateHCID 183913-Methyl-4-(methylthio)phenolHCID 7351522-Chloro-4-nitropyridine

생성물 1

HCID 130736652-Chloro-4-(3-methyl-4-methylmercapto-phenoxy)-pyridine

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

A solution of 17 gm (0.1 mol) of 3-methyl-4-methylmercaptophenol and 15.9 gm (0.1 mol) of 2-chloro-4-nitropyridine in 150 ml of acetonitrile was mixed with 13.8 gm (0.1 mol) of K2CO3 and stirred for 3 hours under reflux. It was then cooled and poured into 300 ml of water. The oil which separated out was separated off and taken up in methylene chloride, and the solution was washed with dilute sodium hydroxide solution and with water. The organic solution was then dried over Na2SO4 and concentrated by evaporation. The oil which remained was crystallized from hexane.

후처리

  1. temperatureunder reflux
  2. temperatureIt was then cooled
  3. customThe oil which separated out
  4. customwas separated off
  5. washthe solution was washed with dilute sodium hydroxide solution and with water
  6. dry with materialThe organic solution was then dried over Na2SO4
  7. concentrationconcentrated by evaporation
  8. customThe oil which remained was crystallized from hexane

출처 및 근거

ORD 기록
ord-1838b3c0eac4477f8df4cdf9a0d5ea63
출처 데이터셋
uspto-grants-1984_06
특허 번호
US04453972

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