5-Chloro-2-nitropyridine → 5-(Methylthio)-2-nitropyridine

HRID 917861노트

반응식

HRID 917861 반응식
Cl[C:2]1[CH:3]=[CH:4][C:5]([N+:8]([O-:10])=[O:9])=[N:6][CH:7]=1.[CH3:11][S-:12].[Na+]>C(O)C>[CH3:11][S:12][C:2]1[CH:3]=[CH:4][C:5]([N+:8]([O-:10])=[O:9])=[N:6][CH:7]=1

참가 물질

4

반응물 2

HCID 2598065-Chloro-2-nitropyridineHCID 4378561Sodium methanethiolate2회

생성물 1

HCID 220361825-(Methylthio)-2-nitropyridine

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

5-Chloro-2-nitropyridine (8.0 grams) was added to a solution of 2.5 grams of sodium methanethiolate in 100 milliliters of ethanol at a temperature of 0°C. to which solution excess sodium methanethiolate was added portionwise. The resulting reaction mixture was then heated to reflux and refluxed for 15 hours with constant stirring. At the end of the 15 hours, the reaction mixture was filtered and allowed to concentrate to 75 milliliters. The reaction mixture was then permitted to cool and filtered again, yielding the desired 5-(methylthio)-2-nitropyridine; it was recrystallized from ethanol, m.p., 100.5°-02.5°C.

후처리

  1. additionwas added portionwise
  2. customThe resulting reaction mixture
  3. temperaturewas then heated
  4. temperatureto reflux
  5. temperaturerefluxed for 15 hours with constant stirring
  6. filtrationAt the end of the 15 hours, the reaction mixture was filtered
  7. concentrationto concentrate to 75 milliliters
  8. temperatureto cool
  9. filtrationfiltered again

출처 및 근거

ORD 기록
ord-d713405093b54466aed4a578972d3764
출처 데이터셋
uspto-grants-1976_07
특허 번호
US03968116

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