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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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HRID 2292028 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])=[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
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참가 물질

4

반응물 2

HCID 70297m-Chloroperbenzoic acidHCID 13936019HCID 13936019, 화합물

생성물 1

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

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-e184bec38aa14531903c79e96f7b8d90
출처 데이터셋
uspto-grants-1989_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04800201

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