Water → 3-Methoxy-5-(trifluoromethyl)phenol

HRID 24701

반응식

HRID 24701 반응식
[CH3:1][O:2][C:3]1[CH:4]=[C:5]([CH:7]=[C:8]([C:10]([F:13])([F:12])[F:11])[CH:9]=1)N.N([O-])=[O:15].[Na+].O>Cl>[CH3:1][O:2][C:3]1[CH:4]=[C:5]([OH:15])[CH:7]=[C:8]([C:10]([F:13])([F:12])[F:11])[CH:9]=1

참가 물질

5

반응물 3

HCID 962WaterHCID 6056715-(Trifluoromethyl)-m-anisidineHCID 23668193Sodium Nitrite

생성물 1

HCID 225717083-Methoxy-5-(trifluoromethyl)phenol

시약·촉매·용매 1

HCID 313Hydrochloric Acid용매

반응 조건

온도
2.5 °C

실험 절차

3-Methoxy-5-(trifluoromethyl)aniline. (5 g) was suspended in 20% HCl (200 mL), stirred for 30 min, cooled to 0-5° C. and diazotized with NaNO2 (2.17 g) added in small portions. The mixture was stirred for 30 min at that temperature and added dropwise to boiling water (200 mL). The mixture was refluxed for 15 min, allowed to cool to room temperature and extracted with AcOEt, dried (MgSO4), filtered and evaporated. The residue was then purified by column chromatography (silica gel; eluent: hexane and AcOEt) to give 3-methoxy-5-(trifluoromethyl)phenol (3.6 g)

후처리

  1. additionadded in small portions
  2. stirringThe mixture was stirred for 30 min at that temperature
  3. additionadded dropwise
  4. temperatureThe mixture was refluxed for 15 min
  5. temperatureto cool to room temperature
  6. extractionextracted with AcOEt
  7. dry with materialdried (MgSO4)
  8. filtrationfiltered
  9. customevaporated
  10. customThe residue was then purified by column chromatography (silica gel; eluent: hexane and AcOEt)

출처 및 근거

ORD 기록
ord-9cde3221516a4fd4859bf0e37d0bf15d
출처 데이터셋
uspto-grants-2005_02
특허 번호
US06855843B2

연결된 노트

불러오는 중…