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Acetic Acid → 5-Chloro-2-(4,4-difluorobut-3-enylsulfonyl)thiazole

HRID 377426
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HRID 377426 반응식
OO.[Cl:3][C:4]1[S:8][C:7]([S:9][CH2:10][CH2:11][CH:12]=[C:13]([F:15])[F:14])=[N:6][CH:5]=1.C(O)(=[O:18])C.[OH-:20].[Na+]>O>[Cl:3][C:4]1[S:8][C:7]([S:9]([CH2:10][CH2:11][CH:12]=[C:13]([F:15])[F:14])(=[O:18])=[O:20])=[N:6][CH:5]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 176Acetic AcidHCID 784Hydrogen PeroxideHCID 14798Sodium HydroxideHCID 11128457HCID 11128457, 화합물

생성물 1

HCID 109566895-Chloro-2-(4,4-difluorobut-3-enylsulfonyl)thiazole수율 82%

시약·촉매·용매 1

HCID 962Water용매

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온도
5 °C

실험 절차

Hydrogen peroxide (0.77 g) was added to a mixture of 5-chloro-2-(4,4-difluorobut-3-enylthio)thiazole (1.94 g) and glacial acetic acid (21 g) at a temperature of 55-60° C. and the resultant mixture maintained at this temperature for 6 hours. After cooling the mixture to 5° C. and adding sufficient 47% sodium hydroxide solution to adjust the pH to 6 the mixture was diluted with water (20 ml) and extracted with chloroform (3×20 ml). The combined extracts were washed with water (20 ml), sodium bisulfite solution (20 ml), and water (20 ml) and dried over anhydrous magnesium sulfate. Removal of the solvent by evaporation under reduced pressure yielded 5-chloro-2-(4,4-difluorobut-3-enylsulfonyl)thiazole (1.95 g, 82%).

후처리

  1. extractionextracted with chloroform (3×20 ml)
  2. washThe combined extracts were washed with water (20 ml), sodium bisulfite solution (20 ml), and water (20 ml)
  3. dry with materialdried over anhydrous magnesium sulfate
  4. customRemoval of the solvent
  5. customby evaporation under reduced pressure

출처 및 근거

ORD 기록
ord-71130ad3f3904317954058b37b70aa69
출처 데이터셋
uspto-grants-2000_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06025497

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