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

HRID 484371노트

반응식

HRID 484371 반응식
[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

참가 물질

3

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온도
0 °C

실험 절차

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).

후처리

  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)

출처 및 근거

ORD 기록
ord-623721c1bfeb4af2aa0bbf9e5ea52ef0
출처 데이터셋
uspto-grants-1993_07
특허 번호
US05231113

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