Sodium → HCID 13682775, 화합물

HRID 231154노트

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HRID 231154 반응식
[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]

참가 물질

5

반응물 3

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

생성물 1

HCID 13682775HCID 13682775, 화합물

시약·촉매·용매 1

HCID 887Methanol용매2회

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-7754fe1fe3c444d8b0c89c8376d0c0ee
출처 데이터셋
uspto-grants-1989_07
특허 번호
US04845118

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