Tris(2-chloroethyl) phosphite → HCID 53993288, compound

Participants

Reaction Steps

13.45 tris-(2-chloroethyl) phosphite and 11.55 grams of the compound of Example 9 dissolved in 50 ml of dry xylene were mixed together and heated at 65° for 3 hours and then at 110° to 115°C for 21/2 hours during which 1,2-dichloroethane distilled out of the reaction mixture and was collected in a trap. The reaction mixture was free of solvent at reduced pressure, the resulting solid was triturated with petroleum ether and then recrystallized successively from a solvent mixture of benzene-hexane and then from toluene, yielding the desired product as white crystals melting at 133° to 135°C (Compound 9).

Provenance & Evidence