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

HRID 1258580ノート

反応式

HRID 1258580 の反応式
[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]

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-2bc57693ea5e458bb7b80e05fb4286e2
出典データセット
uspto-grants-2013_06
特許番号
US08466176B2

反応ノート

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