phosphorous acid, trisodium salt → 5-Cyclopropoxy-2-methylpyridine

HRID 1038578

反応式

HRID 1038578 の反応式
[CH3:1][C:2]1[CH:7]=[CH:6][C:5]([O:8][C:9]2(S(C3C=CC=CC=3)(=O)=O)[CH2:11][CH2:10]2)=[CH:4][N:3]=1.P([O-])([O-])[O-].[Na+].[Na+].[Na+].C(=O)([O-])O.[Na+]>CO.[Na].[Hg]>[CH:9]1([O:8][C:5]2[CH:6]=[CH:7][C:2]([CH3:1])=[N:3][CH:4]=2)[CH2:11][CH2:10]1

参加物

6

反応物 3

HCID 134681phosphorous acid, trisodium saltHCID 516892Sodium BicarbonateHCID 665983222-Methyl-5-[1-(phenylsulfonyl)cyclopropoxy]pyridine

生成物 1

HCID 585206415-Cyclopropoxy-2-methylpyridine収率 86%

試薬・触媒・溶媒 2

HCID 9837419Sodium amalgam触媒HCID 887Methanol溶媒

実験手順

2-Methyl-5-[1-(phenylsulfonyl)cyclopropoxy]pyridine (540 mg, 1.87 mmol) was dissolved in methanol (5.5 mL), added sodium phosphite (671 mg, 5.598 mmol), and sodium amalgam (3.58 g, 7.47 mmol) under ice-cold conditions, stirred at the same temperature for 30 minutes, and then stirred at room temperature for 3 hours. The reaction solution was added a saturated aqueous solution of sodium hydrogen carbonate, and extracted with diethylether. The organic layer was washed with brine, dried over anhydrous sodium sulfate, and concentrated in vacuo. The obtained residue was purified by distillation, and the title compound (240 mg (yield 86%)) was obtained as a yellow oil.

後処理

  1. stirringstirred at room temperature for 3 hours
  2. extractionextracted with diethylether
  3. washThe organic layer was washed with brine
  4. dry with materialdried over anhydrous sodium sulfate
  5. concentrationconcentrated in vacuo
  6. distillationThe obtained residue was purified by distillation

出典と根拠

ORDレコード
ord-2043f59255d14c608041cd6193b3fe29
出典データセット
uspto-grants-2013_10
特許番号
US08551985B2

関連ノート

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