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m-Chloroperbenzoic acid → 2-(3-chlorobenzoyloxy)-5-methyl-6-(4-pyridinyl)-2H-1,4-thiazin-3(4H)-one

HRID 2292030
ノート
印刷プレビュー

反応式

HRID 2292030 の反応式
[Cl:1][C:2]1[CH:7]=[CH:6][CH:5]=[C:4]([C:8]([O:10]O)=[O:9])[CH:3]=1.[CH3:12][C:13]1[NH:14][C:15](=[O:25])[CH2:16][S:17][C:18]=1[C:19]1[CH:24]=[CH:23][N:22]=[CH:21][CH:20]=1>ClCCl>[Cl:1][C:2]1[CH:3]=[C:4]([CH:5]=[CH:6][CH:7]=1)[C:8]([O:10][CH:16]1[C:15](=[O:25])[NH:14][C:13]([CH3:12])=[C:18]([C:19]2[CH:20]=[CH:21][N:22]=[CH:23][CH:24]=2)[S:17]1)=[O:9]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 70297m-Chloroperbenzoic acidHCID 30625322H-1,4-Thiazin-3(4H)-one, 5-methyl-6-(4-pyridinyl)-

生成物 1

HCID 139360302-(3-chlorobenzoyloxy)-5-methyl-6-(4-pyridinyl)-2H-1,4-thiazin-3(4H)-one収率 37.6%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

m-Chloroperbenzoic acid (8.97 g, 70% purity) was added to a solution of 5-methyl-6-(4-pyridinyl)-2H-1,4-thiazin-3(4H)-one (5.0 g) in dichloromethane (120 ml) under ice/water-cooling and the mixture was stirred for 10 minutes under ice/water-cooling. The mixture was washed with saturated sodium bicarbonate aqueous solution (2 times) and successively with water (1 time) and was dried over magnsium sulfate. The solvent was removed under reduced pressure and the residue was recrystallized from ether-petrolem ether to give the titled compound (3.29 g, yield 37.6%) as pale yellow needles.

後処理

  1. temperaturecooling
  2. temperaturecooling
  3. washThe mixture was washed with saturated sodium bicarbonate aqueous solution (2 times) and successively with water (1 time)
  4. dry with materialwas dried over magnsium sulfate
  5. customThe solvent was removed under reduced pressure
  6. customthe residue was recrystallized from ether-petrolem ether

出典と根拠

ORDレコード
ord-d72e1f4673334960b9298eb2c670d763
出典データセット
uspto-grants-1989_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04800201

反応ノート

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