1H,1H-PERFLUORO-3,6-DIOXADECAN-1-OL synthesis

Yield:-

Reaction Conditions:

with sodium borohydrid;sulfuric acid in methanol;water;

Steps:

3 EXAMPLE 3

EXAMPLE 3 Sodium borohydride (8.3 g) was added to a flask fitted with a condenser, overhead stirrer, thermometer, and addition funnel. The sodium borohydride was slurried with tetraglyme (100 g). With good stirring, methyl perfluoro-2-(butoxyethoxy)acetate (100 g, prepared by fluorination and methanolysis of butoxyethoxyethyl acetate) was added over a 30 minute period. The reaction mixture was heated at 90° C. for two hours and then cooled to 40° C. Methanol (18 g) was added slowly. The reaction mixture was heated at 50° C. for 30 minutes, then water (160 g) was rapidly added. After the addition of the water was complete, concentrated sulfuric acid (11 g) was added to the water/product mixture. The crude product was washed with water (160 g) to yield 95 g crude product. The crude product was distilled at 160 Pa (1.2 mm Hg) at a head temperature of 51°-60° C. to give 77.8 g of the desired product, 1,1-dihydroperfluoro-2-(butoxyethoxy) ethanol.

References:

US5437812,1995,A US5482650,1996,A