Pentaerythritol → Pentaerythritol, cyclic phosphate (1:1) (8CI)
反応式
[OH:1][CH2:2][C:3]([CH2:8][OH:9])([CH2:6][OH:7])[CH2:4][OH:5].[P:10](Cl)(Cl)(Cl)=[O:11]>CC(C1C=CC(OP(OC2C=CC=CC=2)(OC2C=CC=CC=2)=O)=CC=1)C.CC(C1C=CC=C(OP(OC2C=CC=CC=2)(OC2C=CC=CC=2)=O)C=1)C.CC(C1C(OP(OC2C=CC=CC=2)(OC2C=CC=CC=2)=O)=CC=CC=1)C>[CH2:4]1[O:5][P:10]2([O:7][CH2:6][C:3]1([CH2:8][OH:9])[CH2:2][O:1]2)=[O:11]参加物
4
反応条件
- 温度
- 100 °C
実験手順
In a 250 mL four-necked reaction flask fitted with a mechanical stirrer, pot thermometer, addition funnel, and condenser with gas outlet were placed 42.5 g (0.313 mole) of pentaerythritol and 150 mL of PHOSFLEX 41P brand of isopropylated triphenyl phosphate under nitrogen. The mixture was stirred and heated at 95° C. as 49.2 g (0.321 mole) of phosphorus oxychloride was added dropwise over five hours. The resulting white slurry was heated to 100° C. with a nitrogen gas sparge for eight hours to remove HCl. The mixture was cooled to 50° C. and filtered. The solid was washed three times with 40 mL of hexane and dried at 100° C./2 mm Hg for sixteen hours to give 42.3 g (71.2% yield) of crude pentaerythritol phosphate alcohol (2,6,7-trioxa- 1-phosphabicyclo [2.2.2]octane-4-methanol-1-oxide). The product had a 31P NMR resonance at -6.0 ppm in d6 -DMSO.