Dimethylamine → Diethyl ((3,5-bis(1,1-dimethylethyl)-4-hydroxyphenyl)methyl)phosphonate

Participants

Reaction Conditions

Reaction Steps

3.2 g of HTMP (hydroxymethylpiperidine), 52.3 g of paraformaldehyde and 206.3 g of 2,6-di-tert-butylphenol are rendered inert and are initially introduced at 60° C. under reduced pressure into a double-jacketed flask with an outlet at the bottom, a baffle, an impeller stirrer and a sublevel air lock for gas introduction. 52 g of dimethylamine gas are introduced at this temperature and the mixture is stirred at 85° C. for 1 hour. Addition of 332 g of triethyl phosphite is then carried out, after which the reaction mixture is kept at 115° C. for 4 hours. Working-up: distillation of triethyl phosphite and dimethylamine under reduced pressure and crystallization of the residue from ligroin yield 320 g of product (90%), melting point 114° C.

Provenance & Evidence