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

HRID 917861ノート

反応式

HRID 917861 の反応式
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

参加物

4

反応物 2

HCID 2598065-Chloro-2-nitropyridineHCID 4378561Sodium methanethiolate2 回

生成物 1

HCID 220361825-(Methylthio)-2-nitropyridine

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-d713405093b54466aed4a578972d3764
出典データセット
uspto-grants-1976_07
特許番号
US03968116

反応ノート

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