Acetone → 2-Methyl-1-(3-trifluoromethyl-phenyl)-propan-2-ol

HRID 866409

반응식

HRID 866409 반응식
[F:1][C:2]([F:12])([F:11])[C:3]1[CH:4]=[C:5]([CH:8]=[CH:9][CH:10]=1)[CH2:6]Cl.[Mg].[CH3:14][C:15]([CH3:17])=[O:16].Cl>CCOCC>[F:1][C:2]([F:12])([F:11])[C:3]1[CH:4]=[C:5]([CH2:6][C:15]([CH3:17])([OH:16])[CH3:14])[CH:8]=[CH:9][CH:10]=1

참가 물질

6

반응물 4

HCID 180AcetoneHCID 313Hydrochloric AcidHCID 697163-(Trifluoromethyl)benzyl chlorideHCID 5462224Magnesium

생성물 1

HCID 149749932-Methyl-1-(3-trifluoromethyl-phenyl)-propan-2-ol수율 73%

시약·촉매·용매 1

HCID 3283Diethyl Ether용매

실험 절차

A solution of 3-trifluoromethylbenzyl chloride (25.0g; 0.128 mole) in ether (130 ml) was added dropwise during 50 minutes to magnesium (3.11 g; 0.128 mole) in a three-necked dry flask equipped with stirrer and reflux condenser. The spontaneous reflux was allowed to continue for another half an hour. The solution was cooled and acetone (7.45; 0.128 mole) was added dropwise (8 minutes) and the solution heated to reflux for three hours. After cooling the reaction mixture was poured out on ice (100 ml) and concentrated hydrochloric acid (11 ml). The phases were separated. The organic phase was washed with water, dried (Na2SO4) and evaporated in vacuum. The residual oil was fractioned affording 1-(3-trifluoromethylphenyl)-2-methyl-2-propanol. (B.p. 63°-64° C/1.0 mm Hg, M.p. 55°-56° C recryst. from petroleum ether.) Yield: 73%; 20.3 g.

후처리

  1. customequipped with stirrer
  2. temperaturereflux condenser
  3. temperatureThe spontaneous reflux
  4. waitto continue for another half an hour
  5. temperatureThe solution was cooled
  6. temperaturethe solution heated
  7. temperatureto reflux for three hours
  8. temperatureAfter cooling the reaction mixture
  9. customThe phases were separated
  10. washThe organic phase was washed with water
  11. dry with materialdried (Na2SO4)
  12. customevaporated in vacuum

출처 및 근거

ORD 기록
ord-e975e732fbb94d9da67a846f222ff03b
출처 데이터셋
uspto-grants-1978_07
특허 번호
US04098901

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