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

HRID 866409

反応式

HRID 866409 の反応式
[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

参加物

6

反応物 4

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-e975e732fbb94d9da67a846f222ff03b
出典データセット
uspto-grants-1978_07
特許番号
US04098901

関連ノート

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