Potassium Carbonate → 2-(1,3-Dioxolan-2-yl)-6-methylpyridine 1-oxide

HRID 1258580노트

반응식

HRID 1258580 반응식
[O:1]1[CH2:5][CH2:4][O:3][CH:2]1[C:6]1[CH:11]=[CH:10][CH:9]=[C:8]([CH3:12])[N:7]=1.C1C=C(Cl)C=C(C(OO)=[O:21])C=1.C([O-])([O-])=O.[K+].[K+]>C(Cl)Cl>[O:1]1[CH2:5][CH2:4][O:3][CH:2]1[C:6]1[CH:11]=[CH:10][CH:9]=[C:8]([CH3:12])[N+:7]=1[O-:21]

참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 70297m-Chloroperbenzoic acidHCID 27343042-(1,3,-Dioxolan-2-yl)-6-methylpyridine

생성물 1

HCID 671899662-(1,3-Dioxolan-2-yl)-6-methylpyridine 1-oxide수율 84.5%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

To a solution 2-(1,3-dioxolan-2-yl)-6-methylpyridine (3.7 g, 15.67 mmol, 1 eq.) in 200 ml of DCM was added mCPBA (7.21 g, 31.35 mmol, 2 eq.) portionwise (exotherm 20° C.>26° C.). The reaction was stirred for 1 hr and 100 ml of 2M aqueous K2CO3 solution was added. The mixture was stirred for 15 mins and the organic layer was separated, washed with water (100 ml), dried over MgSO4 and evaporated to give 2-(1,3-dioxolan-2-yl)-6-methylpyridine 1-oxide (2.4 g, 80% yield) as a yellow liquid.

후처리

  1. stirringThe mixture was stirred for 15 mins
  2. customthe organic layer was separated
  3. washwashed with water (100 ml)
  4. dry with materialdried over MgSO4
  5. customevaporated

출처 및 근거

ORD 기록
ord-2bc57693ea5e458bb7b80e05fb4286e2
출처 데이터셋
uspto-grants-2013_06
특허 번호
US08466176B2

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