m-Chloroperbenzoic acid → 2-(Chloromethyl)-3-(methoxycarbonyl)pyridine 1-oxide

HRID 2277614ノート

反応式

HRID 2277614 の反応式
[CH3:1][O:2][C:3](=[O:12])[C:4]1[CH:9]=[CH:8][CH:7]=[N:6][C:5]=1[CH2:10][Cl:11].C1C=C(Cl)C=C(C(OO)=[O:21])C=1>C(Cl)Cl>[Cl:11][CH2:10][C:5]1[C:4]([C:3]([O:2][CH3:1])=[O:12])=[CH:9][CH:8]=[CH:7][N+:6]=1[O-:21]

参加物

4

反応物 2

HCID 70297m-Chloroperbenzoic acidHCID 19081344Methyl 2-(chloromethyl)pyridine-3-carboxylate

生成物 1

HCID 582166522-(Chloromethyl)-3-(methoxycarbonyl)pyridine 1-oxide収率 92%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

To a stirred solution of methyl-2-(chloromethyl)nicotinate (20 g, 108 mmol) in DCM (300 mL) was added m-CPBA (20.5 g, 119 mmol) at 0° C. After it was stirred at room temperature for 16 hours, the reaction mixture was washed with a mixture of satd. aq. Na2SO3 and NaHCO3 solution. The organic layer was dried over anhy. Na2SO4, filtered, and concentrated in vacuo to give the crude title product (20 g, yield 92%), which was used in the next step reaction without further purification.

後処理

  1. washthe reaction mixture was washed with a mixture of satd
  2. customThe organic layer was dried over anhy
  3. filtrationNa2SO4, filtered
  4. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-da39907af2fc4546bdc2558c6b94d518
出典データセット
uspto-grants-2015_09
特許番号
US09133158B2

反応ノート

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