Sodium → HCID 13682775、化合物

HRID 231154ノート

反応式

HRID 231154 の反応式
[CH3:1][O-:2].[Na+].[Na].[Cl:5][C:6]1[C:11](Cl)=[CH:10][CH:9]=[N+:8]([O-:13])[C:7]=1[CH3:14]>CO>[Cl:5][C:6]1[C:11]([O:2][CH3:1])=[CH:10][CH:9]=[N+:8]([O-:13])[C:7]=1[CH3:14]

参加物

5

反応物 3

HCID 5360545SodiumHCID 10942334Sodium MethoxideHCID 136827893,4-Dichloro-2-methyl-1-oxo-1lambda~5~-pyridine

生成物 1

HCID 13682775HCID 13682775、化合物

試薬・触媒・溶媒 1

HCID 887Methanol溶媒2 回

実験手順

To a solution of sodium methylate, prepared from 0.51 g of sodium and 20 ml of methanol, at -10° C. were added 3.5 g of 3,4-dichloro-2-picoline-N-oxide in 20 ml of anhydrous methanol. The mixture was allowed to warm slowly to room temperature and was then heated to reflux for 1 hour. The solvent was now removed by distillation under reduced pressure, water was added to the residue, the mixture was extracted with dichloromethane, and the solvent was evaporated off. Colorless crystals from diisopropyl ether, melting point 94°-97° C.

後処理

  1. temperaturewas then heated
  2. temperatureto reflux for 1 hour
  3. customThe solvent was now removed by distillation under reduced pressure, water
  4. additionwas added to the residue
  5. extractionthe mixture was extracted with dichloromethane
  6. customthe solvent was evaporated off

出典と根拠

ORDレコード
ord-7754fe1fe3c444d8b0c89c8376d0c0ee
出典データセット
uspto-grants-1989_07
特許番号
US04845118

反応ノート

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