Sodium Hydroxide → HCID 67279950、化合物

HRID 1693336ノート

反応式

HRID 1693336 の反応式
[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]

参加物

6

反応物 4

HCID 14798Sodium HydroxideHCID 24813Phosphorus oxychlorideHCID 516892Sodium BicarbonateHCID 67280656HCID 67280656、化合物

生成物 1

HCID 67279950HCID 67279950、化合物

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-29b449628fba427cb5f1b54f09d9e94a
出典データセット
uspto-grants-2012_04
特許番号
US08158638B2

反応ノート

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