Methanol → Pyridine, 2-(methylthio)-3-nitro-

HRID 22881

반응식

HRID 22881 반응식
CO.Cl[C:4]1[C:9]([N+:10]([O-:12])=[O:11])=[CH:8][CH:7]=[CH:6][N:5]=1.[CH3:13][S-:14].[Na+]>O>[CH3:13][S:14][C:4]1[C:9]([N+:10]([O-:12])=[O:11])=[CH:8][CH:7]=[CH:6][N:5]=1

참가 물질

5

반응물 3

HCID 887Methanol2회HCID 796132-Chloro-3-nitropyridineHCID 4378561Sodium methanethiolate

생성물 1

HCID 572042Pyridine, 2-(methylthio)-3-nitro-수율 64%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

A methanol (50 ml) solution of 2-chloro-3-nitropyridine (4.30 g, 27.1 mmol) was added dropwise to a methanol (30 ml) solution of sodium thiomethoxide (2.10 g, 28.5 mmol) while being cooled with ice, and the mixed solution was stirred for 17 hours. Water was then added to the reaction mixture, and the resulting mixture was extracted with ethyl acetate. The organic layer was washed with a saturated aqueous solution of sodium chloride, and dried over sodium sulfate. Subsequently, the solvent was distilled off, and the resulting crystals were recrystallized from a mixture of an ethyl acetate-hexane mixture to obtain 2.93 g (yield 64%) of 2-methylthio-3-nitropyridine as a yellow needle crystal.

후처리

  1. temperaturewhile being cooled with ice
  2. extractionthe resulting mixture was extracted with ethyl acetate
  3. washThe organic layer was washed with a saturated aqueous solution of sodium chloride
  4. dry with materialdried over sodium sulfate
  5. distillationSubsequently, the solvent was distilled off
  6. customthe resulting crystals were recrystallized from a mixture of an ethyl acetate-hexane mixture

출처 및 근거

ORD 기록
ord-7257ee8926b142a19f5f9af085d27b45
출처 데이터셋
uspto-grants-2005_02
특허 번호
US06849647B1

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