2-Hydroxy-2-methyl-5-phenylpentane → 1,1-Dimethyl-1,2,3,4-tetrahydronaphthalene

HRID 484371

反応式

HRID 484371 の反応式
[CH3:1][C:2](O)([CH2:4][CH2:5][CH2:6][C:7]1[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=1)[CH3:3]>O>[CH3:1][C:2]1([CH3:3])[C:12]2[C:7](=[CH:8][CH:9]=[CH:10][CH:11]=2)[CH2:6][CH2:5][CH2:4]1

参加物

3

反応物 1

HCID 3464292-Hydroxy-2-methyl-5-phenylpentane

生成物 1

HCID 161371,1-Dimethyl-1,2,3,4-tetrahydronaphthalene

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
0 °C

実験手順

To 18 ml of ice-cold concentrated H2SO4 was added 17.8 g (0.1 mol) of 2-methyl-5-phenyl-2-pentanol over 10 minutes. The mixture was then stirred at 0° C. for 15 minutes and at room temperature for 15 minutes. The mixture was treated with 50 ml of water and then extracted with ether. The ether extracts were combined and washed with water and saturated NaCl and NaHCO3 solutions and then dried (MgSO4). The solution was filtered and the solvent removed in-vacuo. The residue was purified by distillation (93° C.; 10 mm) to give the title compound as a colorless oil. PMR (CDCl3): δ 1.19 (6H, s), 1.45-1.53 (2H, m), 1.62-1.73 (2H, m), 2.62 (2H, t, J~6.1 Hz), 7.14-7.30 (4H, m).

後処理

  1. extractionextracted with ether
  2. washwashed with water and saturated NaCl and NaHCO3 solutions
  3. dry with materialdried (MgSO4)
  4. filtrationThe solution was filtered
  5. customthe solvent removed in-vacuo
  6. distillationThe residue was purified by distillation (93° C.; 10 mm)

出典と根拠

ORDレコード
ord-623721c1bfeb4af2aa0bbf9e5ea52ef0
出典データセット
uspto-grants-1993_07
特許番号
US05231113

関連ノート

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