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

HRID 631817

반응식

HRID 631817 반응식
[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]

참가 물질

4

반응물 2

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

생성물 1

HCID 124874842-Chloro-4-methylpyridine 1-oxide수율 88.8%

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

반응 조건

온도
0 °C

실험 절차

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]+.

후처리

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

출처 및 근거

ORD 기록
ord-8377b7d595bc4d13b1e0b8a8fc18f5b2
출처 데이터셋
uspto-grants-2016_04
특허 번호
US09321724B2

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