Preparation of IV is attended by extreme lachrymatory effects. All operations should be carried out in a hood, and with a gas mask and rubber gloves. Freshly prepared phosphorus pentabromide (295 g., 0.685 mole) and 121.8 g.(0.685 mole) of purified anhydrous l, l, l- trichloro-2-methyl-2-propanol (I) were mixed in a flask bearing a drying tube, and heated at 100'for 8 hours. The anhydrous reaction mixture and became dark amber in color and was ...
