Phosphorus tribromide → 6-Methoxy-3-(trifluoromethyl)indene

HRID 2269270노트

반응식

HRID 2269270 반응식
O[C:2]1([C:13]([F:16])([F:15])[F:14])[C:10]2[C:5](=[CH:6][C:7]([O:11][CH3:12])=[CH:8][CH:9]=2)[CH2:4][CH2:3]1.P(Br)(Br)Br>O>[CH3:12][O:11][C:7]1[CH:6]=[C:5]2[C:10]([C:2]([C:13]([F:14])([F:15])[F:16])=[CH:3][CH2:4]2)=[CH:9][CH:8]=1

참가 물질

4

반응물 2

HCID 24614Phosphorus tribromideHCID 186776465-methoxy-1-(trifluoromethyl)-2,3-dihydro-1H-inden-1-ol

생성물 1

HCID 186776456-Methoxy-3-(trifluoromethyl)indene수율 93%

시약·촉매·용매 1

HCID 962Water용매

반응 조건

온도
80 °C

실험 절차

To a stirred Compound 62(850 mg, 3.66 mmol) was added PBr3(9.90 g, 36.6 mmol) with ice-cooling. The reaction mixture was stirred at 80° C. for 6 h. The mixture was diluted with water with ice-cooling and extracted with CH2Cl2. The combined solution was washed with sat. NaHCO3 and brine, dried(MgSO4) and concentrated in vacuo to give crude product as a yellow oil. The crude product was purified by column chromatography on silica gel with hexane-ethyl acetate(50:1-40:1) to give Compound 63(727 mg, 93%) as a yellow oil.

후처리

  1. temperaturecooling
  2. temperaturecooling
  3. extractionextracted with CH2Cl2
  4. washThe combined solution was washed with sat. NaHCO3 and brine, dried(MgSO4)
  5. concentrationconcentrated in vacuo
  6. customto give crude product as a yellow oil
  7. customThe crude product was purified by column chromatography on silica gel with hexane-ethyl acetate(50:1-40:1)

출처 및 근거

ORD 기록
ord-a9e2f4e3c5da4db79fe46389811f355c
출처 데이터셋
uspto-grants-2001_12
특허 번호
US06329396B1

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