Formaldehyde → Dibenzyl (hydroxymethyl)phosphonate
反応式
[P:1]([O-:18])([O:10][CH2:11][C:12]1[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=1)[O:2][CH2:3][C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][CH:5]=1.[CH2:19]=[O:20]>C(N(CC)CC)C>[OH:20][CH2:19][P:1](=[O:18])([O:10][CH2:11][C:12]1[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=1)[O:2][CH2:3][C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][CH:5]=1参加物
4
反応条件
- 温度
- 55 °C
実験手順
100 ml of dibenzyl phosphite, 12.5 g of paraformaldehyde and 6.2 ml of triethylamine were mixed together with stirring. On slow warming to 55° C., a temperature increase to 120° C. took place. The solution, which was now clear, was allowed to cool to 90° C. and was stirred at this temperature for a further 30 minutes. After cooling to room temperature, it was chromatographed on 1 kg of silica gel at elevated pressure (eluent: n-hexane/ethyl acetate 1:4). After concentrating the fractions and drying the residue in vacuo at 60° C. for 12 hours, 96.1 g of pure, oily dibenzyl hydroxymethylphosphonate were obtained, which was reacted without further purification.