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

HRID 1381900노트

반응식

HRID 1381900 반응식
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

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-b9a8df7e12b347659a93d414bcbb4014
출처 데이터셋
uspto-grants-1989_02
특허 번호
US04804668

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