Diethylphosphite → HCID 178527008, compound

Temperature

135 °C

3,9-Dioxo-3,9-diphospha-2,4,8,10-tetraoxa-spiro[5.5]undecane was prepared as follows. Under stirring and a nitrogen atmosphere a suspension of 68 g of pentaerythitol, 152 g of diethylphosphite, and 73 g of water-free tetraline was heated to 135° C. At 135° C., 55% of the theoretical amount of ethanol were removed from the reaction mixture over a period of 3 h. The pressure was diminished slowly to 10 kPa and more ethanol was removed at 135° C. After cooling to 80° C., 60 g of methanol were added after which the methanol layer with the product was separated from the tetraline layer. After evaporation at a 95° C. and a pressure of 0.2 kPa, 100 g of a viscous product were obtained, which crystallized on standing at room temperature.

1. customAt 135° C., 55% of the theoretical amount of ethanol were removed from the reaction mixture over a period of 3 h
2. customwas removed at 135° C
3. temperatureAfter cooling to 80° C.
4. addition60 g of methanol were added after which the methanol layer with the product
5. customwas separated from the tetraline layer
6. customAfter evaporation at a 95° C.

ORD record

ord-c4d02eadc1c946ec8379acdc40aee9b1

Source dataset

uspto-grants-2001_09

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US06284869B1