Potassium Carbonate → 2,2-dimethoxy-5-methyl-4H-1,4-thiazin-3-one

HRID 1381900ノート

反応式

HRID 1381900 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])=[CH:16][S:15]1.C(=O)([O-])[O-].[K+].[K+]>CO>[CH3:12][O:13][C:14]1([O:9][CH3:8])[C:19](=[O:20])[NH:18][C:17]([CH3:21])=[CH:16][S:15]1

参加物

5

反応物 3

HCID 11430Potassium CarbonateHCID 70297m-Chloroperbenzoic acidHCID 143697982-methoxy-5-methyl-2H-1,4-thiazin-3(4H)-one

生成物 1

HCID 143697992,2-dimethoxy-5-methyl-4H-1,4-thiazin-3-one収率 53%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

m-Chloroperbenzoic acid (25.6 g) was added dropwise to a stirred solution of 2-methoxy-5-methyl-2H-1,4-thiazin-3(4H)-one (16 g) in methanol (500 ml) under ice-cooling and the mixture was stirred at room temperature for 4 hours. Then, the reaction mixture was made alkaline by addition of anhydrous potassium carbonate and evaporated to dryness. The residue was extracted twice with chloroform and the combined extracts were washed with water, dried over anhydrous magnesium sulfate and evaporated to dryness. The residue was triturated with ethyl ether to give 2,2-dimethoxy-5-methyl-2H-1,4-thiazin-3(4H)-one (10 g, yield 53%) as pale yellow plates.

後処理

  1. temperaturecooling
  2. customevaporated to dryness
  3. extractionThe residue was extracted twice with chloroform
  4. washthe combined extracts were washed with water
  5. dry with materialdried over anhydrous magnesium sulfate
  6. customevaporated to dryness
  7. customThe residue was triturated with ethyl ether

出典と根拠

ORDレコード
ord-b9a8df7e12b347659a93d414bcbb4014
出典データセット
uspto-grants-1989_02
特許番号
US04804668

反応ノート

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