4-Aminothiophenol → 4-(pyridin-3-ylmethylsulfanyl)aniline

HRID 856676노트

반응식

HRID 856676 반응식
[NH2:1][C:2]1[CH:7]=[CH:6][C:5]([SH:8])=[CH:4][CH:3]=1.[OH-].[Na+].Cl.Cl[CH2:13][C:14]1[CH:15]=[N:16][CH:17]=[CH:18][CH:19]=1>CO>[N:16]1[CH:17]=[CH:18][CH:19]=[C:14]([CH2:13][S:8][C:5]2[CH:6]=[CH:7][C:2]([NH2:1])=[CH:3][CH:4]=2)[CH:15]=1

참가 물질

5

반응물 3

HCID 145104-AminothiophenolHCID 14798Sodium HydroxideHCID 233943-(Chloromethyl)pyridine hydrochloride

생성물 1

HCID 36420654-(pyridin-3-ylmethylsulfanyl)aniline수율 75.8%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

4-aminothiophenol (10 g) was dissolved in methanol (200 ml), aqueous solution of sodium hydroxide (15.7 g, 60 ml) was added to the mixture, 3-(chloromethyl)pyridine hydrochloride (14.4 g) was added to the mixture at 0° C., and the mixture was stirred for 2 hours at room temperature. The solvent was removed under reduced pressure, and the obtained residue was added to water, and extracted with ethyl acetate. The organic layer was washed with saturated brine, and dried over magnesium sulfate. The solvent was removed under reduced pressure and the obtained residue was washed with hexane/ethyl acetate, to give 4-[(3-pyridinylmethyl)sulfanyl]aniline (13.1 g).

후처리

  1. additionwas added to the mixture at 0° C.
  2. customThe solvent was removed under reduced pressure
  3. additionthe obtained residue was added to water
  4. extractionextracted with ethyl acetate
  5. washThe organic layer was washed with saturated brine
  6. dry with materialdried over magnesium sulfate
  7. customThe solvent was removed under reduced pressure
  8. washthe obtained residue was washed with hexane/ethyl acetate

출처 및 근거

ORD 기록
ord-51bca4281f294e94a8dc810e41dd71aa
출처 데이터셋
uspto-grants-2007_08
특허 번호
US07262185B2

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