Toluene → HCID 178502922, compound

Temperature

110 °C

To a suitable vessel equipped with a stirring means, a temperature measuring means and a material addition means was charged 11 parts dimethylphenylphosphonite, 2.5 parts methyl iodide and 9 parts toluene. The resultant solution was slowly heated. The reaction is exothermic and the temperature increases to about 110° C., the reaction mixture is maintained at a temperature of about 100°-120° C., and an additional 185 parts dimethylphenylphosphonite slowly added. Additional amounts of methyl iodide, in about 1 part increments, are occasionally added during the phosphonite addition. The reaction mixture was maintained at about 110° C. for an additional hour following the addition of components. The reaction mixture was then distilled collecting the portion boiling at 148°-149° C./17 mm. (96 percent yield of methyl phenylmethylphosphinate). [Harwood and Grisley J. Am. Chem. Soc., 82, 423 (1960)]. ##STR3##

1. customTo a suitable vessel equipped with a stirring means
2. additiona material addition means
3. temperaturethe reaction mixture is maintained at a temperature of about 100°-120° C.
4. temperatureThe reaction mixture was maintained at about 110° C. for an additional hour
5. additionthe addition of components
6. distillationThe reaction mixture was then distilled
7. customcollecting the portion boiling at 148°-149° C./17 mm

ORD record

ord-5e28e03566ac40e9abf270423643f366

Source dataset

uspto-grants-1977_01

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US04005127