반응 #6646

반응 방정식

2-(1,1,3-trimethyl-3-hydroxybutyl) 5-methyl-phenol

Compound 88

2-(1,1,3-trimethyl-3-hydroxybutyl) 5-methyl-phenol

sulfuric acid

→

title compound

2,2,4,4,7-Pentamethyl-chroman

반응 조건

후처리

1. 1
   온도The reaction mixture was heated
2. 2
   온도at reflux for 13 h
3. 3
   온도cooled
4. 4
   기타The organic layer was separated
5. 5
   추출the aqueous layer was extracted with ether
6. 6
   세척washed successively with water, saturated NaHCO3 solution, water again
7. 7
   건조saturated NaCl solution and then dried (MgSO4)
8. 8
   기타The solvent was removed in vacuo

실험 절차

To 2.16 g (11.7 mmol) of 2-(1,1,3-trimethyl-3-hydroxybutyl) 5-methyl-phenol (Compound 88) was added under nitrogen 50 ml of 20% aqueous sulfuric acid. The reaction mixture was heated at reflux for 13 h and then cooled. The organic layer was separated and the aqueous layer was extracted with ether. The organic extracts were combined and washed successively with water, saturated NaHCO3 solution, water again and saturated NaCl solution and then dried (MgSO4). The solvent was removed in vacuo to give the title compound as a yellow oil. PMR (CDCl3) δ 1.32 (6H, s), 1.34 (6H, s), 1.81 (2H, s), 2.26 (3H, s), 6.63 (1H, s), 6.72 (1H, d, J~7.9 Hz), 7.15 (1H, d, J 7.9 Hz).

출처