摘要 |
<p>Preparation of 2,3-dihydro-2,2-dimethyl-7-benzofuranol (I):- Intermediates for 2,3-dihydro-2,2-dimethyl-7-benzofuranyl N-methylcarbamate an insectice. A mixture of 2,3-dihydro-2,2-dimethyl-7-acetyl benzofuran (48 g), CHCl3 (1 l) and 31% peracetic acid in acetic acid (78 ml) was stirred at room temp. for 3 days. The solvent was removed under vacuo; the residue treated with aqueous NaOH (20 g in 250 ml water) and ethanol (25 ml) and refluxed for 2.5 hours. Some of the solvent (50 ml) was distilled off, the residue cooled, neutralised with HCl, extracted with CHCl3 (3 x 30 ml), the residue concentrated in vacuo and the fraction bp 79-90 deg.C/0.3 mm Hg collected as 2,3-dihydro-2,2-dimethyl-7-benzofuranol.</p> |