m-Chloroperbenzoic acid → HCID 21873713, 화합물

HRID 1913433노트

반응식

HRID 1913433 반응식
[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

참가 물질

4

반응물 2

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

생성물 1

HCID 21873713HCID 21873713, 화합물수율 74.8%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

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.

후처리

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

출처 및 근거

ORD 기록
ord-c719cb5409ab47ddaa7edcf1c5aa1156
출처 데이터셋
uspto-grants-2013_12
특허 번호
US08609680B2

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