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

HRID 2277614노트

반응식

HRID 2277614 반응식
[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]

참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-da39907af2fc4546bdc2558c6b94d518
출처 데이터셋
uspto-grants-2015_09
특허 번호
US09133158B2

반응 노트

불러오는 중…