Sodium Hydroxide → HCID 67279950, 화합물

HRID 1693336노트

반응식

HRID 1693336 반응식
[Cl:1][C:2]1[C:3]([CH3:13])=[N+:4]([O-:12])[CH:5]=[C:6]([CH3:11])[C:7]=1[N+]([O-])=O.P(Cl)(Cl)([Cl:16])=O.[OH-].[Na+].C(=O)(O)[O-].[Na+]>ClCCl>[Cl:1][C:2]1[C:3]([CH3:13])=[N+:4]([O-:12])[CH:5]=[C:6]([CH3:11])[C:7]=1[Cl:16]

참가 물질

6

반응물 4

HCID 14798Sodium HydroxideHCID 24813Phosphorus oxychlorideHCID 516892Sodium BicarbonateHCID 67280656HCID 67280656, 화합물

생성물 1

HCID 67279950HCID 67279950, 화합물

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

The above 3-chloro-2,5-dimethyl-4-nitropyridine 1-oxide (405 mg) was dissolved in dichloromethane (5 mL), and phosphorus oxychloride (915 μL) was added with stirring under ice-cooling. After stirring at room temperature overnight, the reaction solution was introduced into ice water and neutralized with 5 N sodium hydroxide and a saturated sodium bicarbonate solution with stirring under ice-cooling. The mixture was extracted with chloroform, and the organic layer was dried over anhydrous magnesium sulfate. The solvent was evaporated under reduced pressure to obtain the title compound (387 mg, quant.) as a solid.

후처리

  1. temperaturecooling
  2. stirringAfter stirring at room temperature overnight
  3. temperaturecooling
  4. extractionThe mixture was extracted with chloroform
  5. dry with materialthe organic layer was dried over anhydrous magnesium sulfate
  6. customThe solvent was evaporated under reduced pressure

출처 및 근거

ORD 기록
ord-29b449628fba427cb5f1b54f09d9e94a
출처 데이터셋
uspto-grants-2012_04
특허 번호
US08158638B2

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