Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | 1-Butanol | HCID 263 | — |
| Reactant | Pyridine | HCID 1049 | — |
| Reactant | Bis(2-methylpropyl) phosphorochloridate | HCID 190219 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 23505277 | HCID 23505277 | — |
Reaction Steps
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).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| Patent number | US06652772B2 |
|---|
| Source dataset | uspto-grants-2003_11 |
|---|
| ORD ID | ord-6fa5472c3fdd4121a4ce7b21b61bec48 |
|---|
| Source note | uspto-grants-2003_11 |
|---|