1-Butanol → HCID 23505277, compound

A solution of diisobutyl chlorophosphate (130.3 g, 0.57 mole) in 600 mL of dichloromethane and 55.37 g (0.70 mole) of pyridine was cooled to 0° C. n-Butanol (42.25 g, 0.57 mole) was added dropwise over 1 hour. The formation of a white precipitate was immediately observed. The reaction mixture was then stirred for 24 hours at room temperature. The pyridinium hydrochloride was filtered off and the solution washed with water (2×250 mL), aqueous 0.5 N HCl (2×250 mL) and water (2×250 mL). The organic phase was dried over anhydrous magnesium sulfate for 12 hours. Filtration of the drying agent, followed by the removal of the solvent using a Roto-vap, yielded n-butyl diisobutyl phosphate as a clear colorless liquid. Distillation of the crude product (68° C. at 0.02 torr) gave 125 g of 96% n-butyl diisobutyl phosphate (BDIBP).

1. additionwas added dropwise over 1 hour
2. filtrationThe pyridinium hydrochloride was filtered off
3. washthe solution washed with water (2×250 mL), aqueous 0.5 N HCl (2×250 mL) and water (2×250 mL)
4. dry with materialThe organic phase was dried over anhydrous magnesium sulfate for 12 hours
5. filtrationFiltration of the drying agent
6. customfollowed by the removal of the solvent

ORD record

ord-42115002b23c47818f7540bc410a3b19

Source dataset

uspto-grants-2001_07

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US06254799B1