Benzyl Chloride → HCID 54220448, compound

Temperature

-70 °C

1.92 g of diethyl 2-butenephosphonate was placed in 10 ml. of dry tetrahydrofuran, and the solution was cooled to -70° C. in an atmosphere of argon. 7 ml. of n-butyl lithium (as a 15% by weight n-hexane solution) was gradually added, and the mixture was stirred at -70° C. for 1 hour. The reaction mixture was turbid assuming a pale yellow color. When 1.7 g of benzyl chloride was added to this mixture, it became clear. The temperature of the reaction mixture was gradually elevated to room temperature, and it was stirred for an additional 2 hours. The reaction mixture was then diluted with dilute hydrochloric acid, and extracted with ether. The extract was washed with a solution of sodium hydrogen carbonate, washed with water, and dried. The solution was concentrated, and then the residue was distilled at reduced pressure to afford 2.33 g of diethyl 1-benzyl-2-butenephosphonate having a boiling point of 144° C. (0.3 mmHg) in a yield of 93%. The analysis values of the product were as follows:

1. customwas gradually elevated to room temperature
2. stirringit was stirred for an additional 2 hours
3. extractionextracted with ether
4. washThe extract was washed with a solution of sodium hydrogen carbonate
5. washwashed with water
6. customdried
7. concentrationThe solution was concentrated
8. distillationthe residue was distilled at reduced pressure

ORD record

ord-dae39785275743b4b4bbe9ff31002b98

Source dataset

uspto-grants-1976_10

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US03988380