Dichloromethane → Dibutyl 2-methylpropyl phosphate

A solution of di-n-butyl chlorophosphate (130.3 g, 0.57 mole) in 600 mL of dichloromethane containing 55.37 g (0.70 mole) of pyridine was cooled to 0° C. Isobutanol (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 was washed with water (2×250 mL), aqueous 0.5 N HCl (2×250 mL) and water (25×250 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 di-n-butyl isobutyl phosphate as a clear colorless liquid. Distillation of the crude product (68° C. at 0.02 torr) gave 125 g of 94.8% di-n-butyl isobutyl phosphate (DBIBP).

1. filtrationThe pyridinium hydrochloride was filtered off
2. washthe solution was washed with water (2×250 mL), aqueous 0.5 N HCl (2×250 mL) and water (25×250 mL)
3. dry with materialThe organic phase was dried over anhydrous magnesium sulfate for 12 hours
4. filtrationFiltration of the drying agent
5. customfollowed by the removal of the solvent

ORD-Eintrag

ord-6e5db12593794fb98219d77019dcd0dd

Quelldatensatz

uspto-grants-2003_11

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US06652772B2