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

HRID 1634733노트

반응식

HRID 1634733 반응식
[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]

참가 물질

5

반응물 2

HCID 70297m-Chloroperbenzoic acidHCID 69987244HCID 69987244, 화합물

생성물 1

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

시약·촉매·용매 2

HCID 6212Chloroform용매HCID 6344Dichloromethane용매

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-ef0f1fa36cca49dfa273a12cc80ab30c
출처 데이터셋
uspto-grants-2003_01
특허 번호
US06506901B2

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