m-Chloroperbenzoic acid → Ethyl 6-(benzenesulphinylmethyl)-3-ethyl-2-methoxybenzoate

HRID 2177688ノート

反応式

HRID 2177688 の反応式
ClC1C=CC=C(C(OO)=[O:9])C=1.[C:12]1([S:18][CH2:19][C:20]2[C:25]([C:26]([O:28][CH2:29][CH3:30])=[O:27])=[C:24]([O:31][CH3:32])[C:23]([CH2:33][CH3:34])=[CH:22][CH:21]=2)[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=1>C(Cl)Cl>[C:12]1([S:18]([CH2:19][C:20]2[C:25]([C:26]([O:28][CH2:29][CH3:30])=[O:27])=[C:24]([O:31][CH3:32])[C:23]([CH2:33][CH3:34])=[CH:22][CH:21]=2)=[O:9])[CH:13]=[CH:14][CH:15]=[CH:16][CH:17]=1

参加物

4

反応物 2

HCID 70297m-Chloroperbenzoic acidHCID 67107436Ethyl 6-(phenylthiomethyl)-3-ethyl-2-methoxybenzoate2 回

生成物 1

HCID 67107367Ethyl 6-(benzenesulphinylmethyl)-3-ethyl-2-methoxybenzoate収率 67.6%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

3-Chloroperbenzoic acid (0.07 g) was added to a stirred solution of ethyl 6-(phenylthiomethyl)-3-ethyl-2-methoxybenzoate (Intermediate 19, 0.315 g) in DCM (5 ml) and the resultant mixture was stirred at room temperature overnight. The solution was evaporated to dryness and the residue was purified by chromatography on silica, eluting with a mixture of ethyl acetate and cyclohexane with a gradient of 0-100% to give ethyl 6-(benzenesulphinylmethyl)-3-ethyl-2-methoxybenzoate (0.095 g) as a clear gum.

後処理

  1. customThe solution was evaporated to dryness
  2. customthe residue was purified by chromatography on silica
  3. washeluting with a mixture of ethyl acetate and cyclohexane with a gradient of 0-100%

出典と根拠

ORDレコード
ord-b4d7d2ca37ba4c18afb332c68cc5581a
出典データセット
uspto-grants-2015_06
特許番号
US09067905B2

反応ノート

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