Chlorodiphenylphosphine → Diphenylphosphine

A THF solution (150 ml) containing chlorodiphenylphosphine (60 g, 0.34 mole) was added dropwise from a dropping flask, and under nitrogen atmosphere to a stirred THF (75 ml) suspension of lithium metal (5 g, 0.7 moles) in a 500 ml round bottom flask. Formation of lithiodiphenylphosphide was indicated by the appearance of a bright red color. After stirring 18 hours, unreacted lithium was removed and the solution was added slowly to a rapidly stirred THF slurry of the brominated resin beads (32 g, 35 percent Br, 131.3 mmol Br). This slurry was allowed to stir two days under nitrogen (longer if high percent Br content resin used). The slurry was then hydrolyzed by adding it to two liters of nitrogen-saturated acetone/water (3:1) and stirring for one hour. The beads were then filtered and washed by stirring successively in one liter each of the following nitrogen-saturated solvents: water (2 hours), acetone (2 hours), benzene/methanol (9:1) (18-24 hours), and methanol (4-5 hours). The beads were then vacuum dried (80° C., 0.05 torr) for 24 hours, and analyzed for 6.44 percent P which corresponds to 35.0 percent of the polystyryl rings substituted with the diphenylphosphide moiety.

1. additionwas added dropwise from a dropping flask
2. customunreacted lithium was removed
3. stirringto stir two days under nitrogen (longer if high percent Br content resin
4. additionby adding it to two liters of nitrogen-saturated acetone/water (3:1)
5. stirringstirring for one hour
6. filtrationThe beads were then filtered
7. washwashed
8. stirringby stirring successively in one liter each of the following nitrogen-saturated solvents
9. customwater (2 hours), acetone (2 hours), benzene/methanol (9:1) (18-24 hours), and methanol (4-5 hours)
10. customvacuum dried (80° C., 0.05 torr) for 24 hours

ORDレコード

ord-74a4e650899e4eea8e3cf265b74afb8c

出典データセット

uspto-grants-1981_03

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US04258206