m-Chloroperbenzoic acid → 2-Chloro-4-methylpyridine 1-oxide

HRID 631817

反応式

HRID 631817 の反応式
[Cl:1][C:2]1[CH:7]=[C:6]([CH3:8])[CH:5]=[CH:4][N:3]=1.C1C=C(Cl)C=C(C(OO)=[O:17])C=1>C(Cl)Cl>[Cl:1][C:2]1[CH:7]=[C:6]([CH3:8])[CH:5]=[CH:4][N+:3]=1[O-:17]

参加物

4

反応物 2

HCID 70297m-Chloroperbenzoic acidHCID 772482-Chloro-4-methylpyridine

生成物 1

HCID 124874842-Chloro-4-methylpyridine 1-oxide収率 88.8%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

反応条件

温度
0 °C

実験手順

2-Chloro-4-methylpyridine (1 g, 7.84 mmol) was dissolved in DCM (10 ml), cooled to 0° C., mCPBA (70%, 2.32 g, 9.41 mmol) was added and the mixture was stirred at 0° C. for several hours and allowed to reach room temperature overnight. The mixture was diluted with DCM and washed with saturated Na2S2O3 solution and saturated sodium bicarbonate solution. After drying (sodium sulfate) and concentration under reduced pressure, 1.0 g of a yellow oil was obtained (6.27 mmol, 80%) MS(ESI) m/z=144.0 [M+1]+.

後処理

  1. washwashed with saturated Na2S2O3 solution and saturated sodium bicarbonate solution
  2. customAfter drying
  3. concentration(sodium sulfate) and concentration under reduced pressure

出典と根拠

ORDレコード
ord-8377b7d595bc4d13b1e0b8a8fc18f5b2
出典データセット
uspto-grants-2016_04
特許番号
US09321724B2

関連ノート

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