Oxalyl chloride → HCID 13353849, compound

Participants

Reaction Steps

A mixture of 127 g (1 mole) of oxalyl chloride, 165 g (1 mole) of perfluoropropyliden-2-imine, and 5 ml of pyridine was heated in a 600 ml Hastelloy tube at 100° for 4 hrs, 150° for 4 hrs, and 200° for 4 hrs. The bomb was cooled and vented, and the contents were filtered to remove suspended solid. Distillation gave 102.3 g of a 25:75 mixture of (CF3)2CClNH2 and the isocyanate, bp 46.0°-46.5°, and 29.3 g of pure isocyanate as a colorless liquid: bp 50.5°-51.0°; 19F nmr (CCl3F) δ 78.0 (s); ir (liquid) 4.40 μ.

Provenance & Evidence