Hydrochloric Acid → 4-{[t-Butyl(diphenyl)silyl]oxy}-3-fluorophenol

HRID 1634734노트

반응식

HRID 1634734 반응식
C([O:4][C:5]1[CH:10]=[CH:9][C:8]([O:11][Si:12]([C:25]([CH3:28])([CH3:27])[CH3:26])([C:19]2[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=2)[C:13]2[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=2)=[C:7]([F:29])[CH:6]=1)(=O)C.[OH-].[Na+].Cl>CO>[Si:12]([O:11][C:8]1[CH:9]=[CH:10][C:5]([OH:4])=[CH:6][C:7]=1[F:29])([C:25]([CH3:28])([CH3:27])[CH3:26])([C:19]1[CH:20]=[CH:21][CH:22]=[CH:23][CH:24]=1)[C:13]1[CH:14]=[CH:15][CH:16]=[CH:17][CH:18]=1

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 699857744-{[t-Butyl(diphenyl)silyl]oxy}-3-fluorophenyl acetate

생성물 1

HCID 699876834-{[t-Butyl(diphenyl)silyl]oxy}-3-fluorophenol수율 95%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

4-{[t -Butyl(diphenyl)silyl]oxy}-3-fluorophenyl acetate (5.28 g, 12.92 mmol) was dissolved in methanol (100 mL). 1N NaOH (15.5 mL) was added. The solution was stirred for 30 minutes at ambient temperature. 1N HCl (16 mL) was added. The solvent was removed in vacuo and the solid partitioned between dichloromethane and water. The aqueous phase was washed with dichloromethane. The organic layers were combined and the solvent dried over anhydrous magnesium sulfate. The solution was filtered and the solvent evaporated to dryness in vacuo to yield crude title compound (4.5 g, 12.28 mmol).

후처리

  1. customThe solvent was removed in vacuo
  2. customthe solid partitioned between dichloromethane and water
  3. washThe aqueous phase was washed with dichloromethane
  4. dry with materialthe solvent dried over anhydrous magnesium sulfate
  5. filtrationThe solution was filtered
  6. customthe solvent evaporated to dryness in vacuo

출처 및 근거

ORD 기록
ord-4e14128c55344091b621e2ece53f2106
출처 데이터셋
uspto-grants-2003_01
특허 번호
US06506901B2

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