m-Chloroperbenzoic acid → HCID 21873713、化合物

HRID 1913433ノート

反応式

HRID 1913433 の反応式
[CH3:1][C:2]1[N:7]=[C:6]2[O:8][CH2:9][CH2:10][O:11][C:5]2=[CH:4][CH:3]=1.C1C=C(Cl)C=C(C(OO)=[O:20])C=1>C(Cl)Cl>[CH3:1][C:2]1[N+:7]([O-:20])=[C:6]2[O:8][CH2:9][CH2:10][O:11][C:5]2=[CH:4][CH:3]=1

参加物

4

反応物 2

HCID 70297m-Chloroperbenzoic acidHCID 156332996-Methyl-2,3-dihydro-[1,4]dioxino[2,3-b]pyridine

生成物 1

HCID 21873713HCID 21873713、化合物収率 74.8%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

To a 0° C. solution of 6-methyl-2,3-dihydro-[1,4]dioxino[2,3-b]pyridine (19 g, 0.12 mol) in anhydrous CH2Cl2 (250 mL) was added m-CPBA (32 g, 0.15 mol) portionwise. The mixture was stirred at room temperature overnight. The solvent was removed in vacuo and the residue was purified via column chromatography (silica gel, EtOAc/petroleum ether 1:1) to yield 6-methyl-2,3-dihydro-[1,4]dioxino[2,3-b]pyridine 5-oxide (15.0 g, 72%) as a white solid.

後処理

  1. customThe solvent was removed in vacuo
  2. customthe residue was purified via column chromatography (silica gel, EtOAc/petroleum ether 1:1)

出典と根拠

ORDレコード
ord-c719cb5409ab47ddaa7edcf1c5aa1156
出典データセット
uspto-grants-2013_12
特許番号
US08609680B2

反応ノート

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