2-(dimethylamino)-4-(trifluoromethyl)-6H-1,3-oxazin-6-one → Ethyl 5-[3,6-dihydro-2,6-dioxo-4-(trifluoromethyl)-1(2H)-pyrimidinyl]-1,2-benzisothiazole-3-acetate

HRID 277379

反応式

HRID 277379 の反応式
[NH2:1][C:2]1[CH:3]=[CH:4][C:5]2[S:9][N:8]=[C:7]([CH2:10][C:11]([O:13][CH2:14][CH3:15])=[O:12])[C:6]=2[CH:16]=1.CN(C)[C:19]1[O:20][C:21](=[O:29])[CH:22]=[C:23]([C:25]([F:28])([F:27])[F:26])[N:24]=1>C(O)(=O)C>[O:20]=[C:19]1[NH:24][C:23]([C:25]([F:26])([F:27])[F:28])=[CH:22][C:21](=[O:29])[N:1]1[C:2]1[CH:3]=[CH:4][C:5]2[S:9][N:8]=[C:7]([CH2:10][C:11]([O:13][CH2:14][CH3:15])=[O:12])[C:6]=2[CH:16]=1

参加物

4

反応物 2

HCID 37238622-(dimethylamino)-4-(trifluoromethyl)-6H-1,3-oxazin-6-oneHCID 11770464Ethyl 5-amino-1,2-benzisothiazole-3-acetate

生成物 1

HCID 10960337Ethyl 5-[3,6-dihydro-2,6-dioxo-4-(trifluoromethyl)-1(2H)-pyrimidinyl]-1,2-benzisothiazole-3-acetate

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

実験手順

A mixture of ethyl 5-amino-1,2-benzisothiazole-3-acetate (0.748 g, 3.16 mmol) and 2-dimethylamino-4-(trifluoromethyl)-6H-1,3-oxazin-6-one (0.660 g, 3.17 mmol) in acetic acid is refluxed for three hours, concentrated in vacuo, and diluted with saturated sodium hydrogen carbonate solution. The resultant mixture is extracted with methylene chloride. The combined organic extracts are washed with water, dried over anhydrous sodium sulfate, and concentrated in vacuo to give the title product as a tan solid which is identified by NMR spectral analysis.

後処理

  1. temperatureis refluxed for three hours
  2. concentrationconcentrated in vacuo
  3. additiondiluted with saturated sodium hydrogen carbonate solution
  4. extractionThe resultant mixture is extracted with methylene chloride
  5. washThe combined organic extracts are washed with water
  6. dry with materialdried over anhydrous sodium sulfate
  7. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-ffa3f6e12c80420e92e029f0313609f4
出典データセット
uspto-grants-2002_03
特許番号
US06355796B1

関連ノート

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