Formaldehyde → HCID 21510427、化合物

反応式

[O:1]([CH2:8][C:9](=[O:14])[C:10]([CH3:13])([CH3:12])[CH3:11])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[CH2:15]=[O:16].[OH-].[Na+]>C(O)C>[OH:16][CH2:15][CH:8]([O:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1)[C:9](=[O:14])[C:10]([CH3:11])([CH3:13])[CH3:12]

参加物

実験手順

1Phenoxy-3,3-dimethyl-butan-2-one (192.2 g, 1.0 mol) prepared according to German Offenlegungsschrift, i.e., (German Published Specification No. 2,105,490; Example 3) and having a boiling point of 75°-83°C at 0.08 atmospheres is dissolved in ethanol (800 ml) and a 30% formaldehyde solution (240 ml, 2.4 mols) is added. A 10% sodium hydroxide solution (5 ml) is then added until the pH is 9. The reaction mixture is heated for 4 hours reflux and the solvent is distilled off in vacuo. The resulting precipitate is filtered off, well rinsed with petroleum ether and discarded. The filtrate is freed from the solvent in vacuo and the resulting oil is taken up in ether and extracted by shaking with water. The organic phase is dried over sodium sulphate and freed from the solvent and the residue is purified by vaccum distillation to afford 145 g (65% of theory) of 1 -hydroxy-2-phenoxy-4,4-dimethyl-pentan-3-one, boiling point 95°-100°C (0.1 mm Hg).