m-Chloroperbenzoic acid → 4-{[t-Butyl(diphenyl)silyl]oxy}-3-fluorophenyl acetate

HRID 1634733ノート

反応式

HRID 1634733 の反応式
[Si:1]([O:18][C:19]1[CH:24]=[CH:23][C:22](C(=O)C)=[CH:21][C:20]=1[F:28])([C:14]([CH3:17])([CH3:16])[CH3:15])([C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.ClC1C=[C:32](C=CC=1)[C:33]([O:35]O)=[O:34]>C(Cl)(Cl)Cl.ClCCl>[C:33]([O:35][C:22]1[CH:23]=[CH:24][C:19]([O:18][Si:1]([C:14]([CH3:16])([CH3:17])[CH3:15])([C:2]2[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=2)[C:8]2[CH:9]=[CH:10][CH:11]=[CH:12][CH:13]=2)=[C:20]([F:28])[CH:21]=1)(=[O:34])[CH3:32]

参加物

5

反応物 2

HCID 70297m-Chloroperbenzoic acidHCID 69987244HCID 69987244、化合物

生成物 1

HCID 699857744-{[t-Butyl(diphenyl)silyl]oxy}-3-fluorophenyl acetate

試薬・触媒・溶媒 2

HCID 6212Chloroform溶媒HCID 6344Dichloromethane溶媒

実験手順

1-(4-{[t-Butyl(diphenyl)silyl]oxy}-3-fluorophenyl)-1-ethanone (8.27 g, 21.07 mmol) was dissolved in chloroform (300 mL). 3-Chloroperoxybenzoic acid (4.0 g, 23.18 mmol) was added and the solution heated to reflux for 72 hours. The solution was diluted with dichloromethane, washed with saturated sodium hydrogen sulfate, saturated sodium hydrogen carbonate, brine and dried over anhydrous magnesium sulfate. The solution was filtered and the solvent evaporated to dryness in vacuo to yield the title compound which was used without further purification (5.28 g, 12.92 mmol).

後処理

  1. temperaturethe solution heated
  2. temperatureto reflux for 72 hours
  3. washwashed with saturated sodium hydrogen sulfate, saturated sodium hydrogen carbonate, brine
  4. dry with materialdried over anhydrous magnesium sulfate
  5. filtrationThe solution was filtered
  6. customthe solvent evaporated to dryness in vacuo

出典と根拠

ORDレコード
ord-ef0f1fa36cca49dfa273a12cc80ab30c
出典データセット
uspto-grants-2003_01
特許番号
US06506901B2

反応ノート

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