Acetic Acid → 6-(5-(Methylsulfonyl)-1,3,4-thiadiazol-2-yl)benzo[d]isothiazole

HRID 2075384ノート

反応式

HRID 2075384 の反応式
[CH3:1][S:2][C:3]1[S:7][C:6]([C:8]2[CH:16]=[CH:15][C:11]3[CH:12]=[N:13][S:14][C:10]=3[CH:9]=2)=[N:5][N:4]=1.OO.CC(O)=[O:21].[OH2:23]>C([O-])(O)=O.[Na+].CCOC(C)=O.[O-][W]([O-])(=O)=O.[Na+].[Na+]>[CH3:1][S:2]([C:3]1[S:7][C:6]([C:8]2[CH:16]=[CH:15][C:11]3[CH:12]=[N:13][S:14][C:10]=3[CH:9]=2)=[N:5][N:4]=1)(=[O:21])=[O:23]

参加物

8

反応物 4

HCID 176Acetic AcidHCID 784Hydrogen PeroxideHCID 962WaterHCID 670892736-(5-(Methylthio)-1,3,4-thiadiazol-2-yl)benzo[d]isothiazole

生成物 1

HCID 670893666-(5-(Methylsulfonyl)-1,3,4-thiadiazol-2-yl)benzo[d]isothiazole

試薬・触媒・溶媒 3

HCID 26052Sodium tungstate触媒HCID 8857Ethyl Acetate溶媒HCID 516892Sodium Bicarbonate溶媒

実験手順

To a stirred mixture of 6-(5-(methylthio)-1,3,4-thiadiazol-2-yl)benzo[d]isothiazole (0.20 g, 0.75 mmol) and hydrogen peroxide (0.19 mL, 1.9 mmol) in AcOH (2.00 mL, 35 mmol) was added sodium tungstate (0.0026 mL, 0.038 mmol). The resulting mixture was stirred at room temperature 16 hours. The mixture was diluted with aqueous NaHCO3 (10 mL), water (10 mL) and EtOAc (5 mL). The separated aqueous layer was extracted with EtOAc (2×10 mL) and the combined organic layers were washed with brine, dried over Na2SO4, and concentrated to give the product as a residue which was used without further purification.

後処理

  1. extractionThe separated aqueous layer was extracted with EtOAc (2×10 mL)
  2. washthe combined organic layers were washed with brine
  3. dry with materialdried over Na2SO4
  4. concentrationconcentrated
  5. customto give the product as a residue which
  6. customwas used without further purification

出典と根拠

ORDレコード
ord-205c70a747cc403b852b076a86733cd7
出典データセット
uspto-grants-2011_04
特許番号
US07919504B2

反応ノート

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