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

HRID 2075384노트

반응식

HRID 2075384 반응식
[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]

참가 물질

8

반응물 4

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

생성물 1

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

시약·촉매·용매 3

HCID 26052Sodium tungstate촉매HCID 8857Ethyl Acetate용매HCID 516892Sodium Bicarbonate용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-205c70a747cc403b852b076a86733cd7
출처 데이터셋
uspto-grants-2011_04
특허 번호
US07919504B2

반응 노트

불러오는 중…