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Peracetic Acid → HCID 53723907、化合物

HRID 1087946
ノート
印刷プレビュー

反応式

HRID 1087946 の反応式
[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
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 6585Peracetic AcidHCID 23665404Sodium Acetate TrihydrateHCID 53653060HCID 53653060、化合物

生成物 1

HCID 53723907HCID 53723907、化合物収率 119.5%

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒

反応条件

温度
60 °C

実験手順

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.

後処理

  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)

出典と根拠

ORDレコード
ord-16ec0bf3edfd4f4ca614ac403df4d15d
出典データセット
uspto-grants-1990_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04960897

反応ノート

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