Methanol → 5-(Methylthio)-2-nitropyridine

HRID 746651노트

반응식

HRID 746651 반응식
CO.Cl[C:4]1[CH:5]=[CH:6][C:7]([N+:10]([O-:12])=[O:11])=[N:8][CH:9]=1.[CH3:13][S-:14].[Na+]>O>[CH3:13][S:14][C:4]1[CH:5]=[CH:6][C:7]([N+:10]([O-:12])=[O:11])=[N:8][CH:9]=1

참가 물질

5

반응물 3

HCID 887Methanol2회HCID 2598065-Chloro-2-nitropyridineHCID 4378561Sodium methanethiolate

생성물 1

HCID 220361825-(Methylthio)-2-nitropyridine수율 45.3%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

A methanol (40 mml) solution of 5-chloro-2-nitropyridine (2.0 g. 12.6 mmol) was added dropwise to a methanol (20 ml) solution of sodium thiomethoxide (1.02 g, 13.9 mmol) while being cooled with ice, and after the mixture was stirred for 13 hours while raising its temperature to the room temperature, water added to the reaction mixture and the mixture was extracted with ethyl acetate. The organic layer was washed with water and then with a saturated aqueous solution of sodium chloride, and dried over magnesium sulfate. Thereafter, the solvent was distilled off, and the resulting crude product was recrystalized with ethyl acetate-hexane to obtain 972 mg (yield 45%) of 5-methylthio-2-nitropyridine.

후처리

  1. temperaturewhile being cooled with ice
  2. additionadded to the reaction mixture
  3. extractionthe mixture was extracted with ethyl acetate
  4. washThe organic layer was washed with water
  5. dry with materialwith a saturated aqueous solution of sodium chloride, and dried over magnesium sulfate
  6. distillationThereafter, the solvent was distilled off
  7. customthe resulting crude product was recrystalized with ethyl acetate-hexane

출처 및 근거

ORD 기록
ord-41afd04ecdd04bf3a0c5a3343c11ceff
출처 데이터셋
uspto-grants-2008_07
특허 번호
US07393866B2

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