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m-Chloroperbenzoic acid → 2,2-Dimethoxy-5-methyl-6-(pyridin-4-yl)-2H-1,4-thiazin-3(4H)-one

HRID 2292028
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反応式

HRID 2292028 の反応式
ClC1C=CC=C([C:8](OO)=[O:9])C=1.[CH3:12][O:13][CH:14]1[C:19](=[O:20])[NH:18][C:17]([CH3:21])=[C:16]([C:22]2[CH:27]=[CH:26][N:25]=[CH:24][CH:23]=2)[S:15]1>CO>[CH3:12][O:13][C:14]1([O:9][CH3:8])[C:19](=[O:20])[NH:18][C:17]([CH3:21])=[C:16]([C:22]2[CH:27]=[CH:26][N:25]=[CH:24][CH:23]=2)[S:15]1
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 13936019HCID 13936019、化合物

生成物 1

HCID 139360292,2-Dimethoxy-5-methyl-6-(pyridin-4-yl)-2H-1,4-thiazin-3(4H)-one収率 66.7%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

m-Chloroperbenzoic acid (2.8 g) was added to a stirred solution of 2 -methoxy-5-methyl-6-(4-pyridinyl)-2H-1,4-thiazin-3(4H)-one (2.7 g) in methanol (100 ml) under ice/water-cooling. The reaction mixture was further stirred at ambient temperature for 2 hours. Methanol was removed under reduced pressure and the residue was dissolved in ethyl acetate, was washed with saturated sodium bicarbonate aqueous solution and successively with water, and was dried over magnesium sulfate. Ethyl acetate was removed under reduced pressure and the residue was crystallized from ether to give the titled compound (2 g, yield 66.7%) as pale yellow powder.

後処理

  1. temperaturecooling
  2. customMethanol was removed under reduced pressure
  3. dissolutionthe residue was dissolved in ethyl acetate
  4. washwas washed with saturated sodium bicarbonate aqueous solution and successively with water
  5. dry with materialwas dried over magnesium sulfate
  6. customEthyl acetate was removed under reduced pressure
  7. customthe residue was crystallized from ether

出典と根拠

ORDレコード
ord-e184bec38aa14531903c79e96f7b8d90
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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