Acetic Acid → HCID 54319289, compound

Participants

Reaction Steps

When a mixture of 32.3 g of tris(2-chloroethyl phosphite, 5.8 g of freshly distilled acetaldehyde, 22.0 g of p-chlorobenzenesulfonamide, and 3.0 g of acetic acid in 100 g of chlorobenzene is stirred and warmed, heat of reaction is observed at about 90°. The temperature is kept at 95°-103° for 1 hr, and then the solvent and by-product are removed at reduced pressure. Ether is added to the residue, causing a solid to separate. This is washed with water and recrystallized from isopropyl alcohol, giving 12.4 g of white solid product: mp 94.5°-98°; 31P nmr (DMSO-d6)- 24.0 ppm.

Provenance & Evidence