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Peracetic Acid → HCID 53723907, 화합물

HRID 1087946
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HRID 1087946 반응식
[CH3:1][N:2]([CH2:14][C:15]([C:17]1[CH:22]=[CH:21][CH:20]=[C:19]([C:23]([F:26])([F:25])[F:24])[N:18]=1)=[CH2:16])[S:3]([CH:6]=[CH:7][C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1)(=[O:5])=[O:4].O.O.O.C([O-])(=[O:32])C.[Na+].C(OO)(=O)C>C(Cl)(Cl)Cl>[O:32]1[C:15]([C:17]2[CH:22]=[CH:21][CH:20]=[C:19]([C:23]([F:25])([F:24])[F:26])[N:18]=2)([CH2:14][N:2]([CH3:1])[S:3]([CH:6]=[CH:7][C:8]2[CH:9]=[CH:10][CH:11]=[CH:12][CH:13]=2)(=[O:4])=[O:5])[CH2:16]1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 6585Peracetic AcidHCID 23665404Sodium Acetate TrihydrateHCID 53653060HCID 53653060, 화합물

생성물 1

HCID 53723907HCID 53723907, 화합물수율 119.5%

시약·촉매·용매 1

HCID 6212Chloroform용매

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온도
60 °C

실험 절차

A mixture of 1.1 g of 3-(N-methyl-N-styrylsulfonylamino)-2-(6-trifluoromethylpyridin-2-yl)propene, 0.20 g of sodium acetate trihydrate, 2.19 g of 40% peracetic acid and 11 ml of chloroform was stirred at 60° C. for 5 hours. After the reaction mixture was cooled to room temperature, 10 ml of carbon tetrachrolide was added thereto, and the whole mixture was subsequently washed with water, an aqueous solution of 10% sodium bisulfite, a 2N aqueous solution of sodium hydroxide, water and saturated saline solution in that order and dried over anhydrous magnesium sulfate. After the solvent was distilled off, the residue was purified by silica gel column chromatography (eluted with benzene-ethyl acetate 15:1) to obtain 0.70 g of Compound No. 4 in Table 1.

후처리

  1. temperatureAfter the reaction mixture was cooled to room temperature
  2. addition10 ml of carbon tetrachrolide was added
  3. washthe whole mixture was subsequently washed with water
  4. dry with materialan aqueous solution of 10% sodium bisulfite, a 2N aqueous solution of sodium hydroxide, water and saturated saline solution in that order and dried over anhydrous magnesium sulfate
  5. distillationAfter the solvent was distilled off
  6. customthe residue was purified by silica gel column chromatography (eluted with benzene-ethyl acetate 15:1)

출처 및 근거

ORD 기록
ord-16ec0bf3edfd4f4ca614ac403df4d15d
출처 데이터셋
uspto-grants-1990_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04960897

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