Phenethyl bromide → Diethyl 2-phenylethyl phosphonate

温度

-15 °C

Diethyl phosphite (27.64 g, 200 m mole) was dissolved in DMF (200 ml), and to the solution at nitrogen atmosphere while stirring and -15° C., sodium hydride (60% in oil, 9.6 g, 220 m mole) was added. The mixture was stirred for 1 hour at not more than 0° C. To the solution phenethyl bromide (37.0 g, 200 m mole) was dropwise added and further the mixture was stirred overnight at room temperature. The DMF solution was distilled under reduced pressure leaving a residue, and the residue was dissolved in ethyl acetate. The ethyl acetate solution was washed with water, and dried with anhydrous sodium sulfate. The solvent was evaporated and the thus obtained oily product was distilled under reduced pressure to obtain diethylphenethylphosphonate (25.0 g, yield: 51.6%) of boiling point 136.5°~137.5° C./3 mmHg.

1. stirringThe mixture was stirred for 1 hour at not more than 0° C
2. stirringfurther the mixture was stirred overnight at room temperature
3. distillationThe DMF solution was distilled under reduced pressure
4. customleaving a residue
5. washThe ethyl acetate solution was washed with water
6. dry with materialdried with anhydrous sodium sulfate
7. customThe solvent was evaporated
8. distillationthe thus obtained oily product was distilled under reduced pressure

ORDレコード

ord-6cdc5fd140114cde9c4f1e2190f32365

出典データセット

uspto-grants-1986_05

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US04590178