Ammonia → HCID 54217769, compound

Participants

Reaction Steps

To a 0° C. solution of 25.1 g (0.16 mol) of POCl3 in 100 mL of dry ether was added a solution of 10.6 g (0.105 mol) of triethylamine in 15 mL of ether over a period of 10 min followed by the cautious addition of 10.8 g (0.10 mol) benzyl alcohol in 15 mL of ether over a period of 0.5 hr at 0.10° C. The solution was stirred for 60 min. and filtered. The volatiles were removed under reduced pressures to provide 26.5 g of a crude oil. The product was treated with NH3 (12 g) in 150 mL of CH2Cl2 at -30° C. After warming to room temperature, the mixture was filtered to provide 28 gm of a solid material. The impure product was washed with water followed by a methanol washing. After drying the product had a mp of 166°-167° C.

Provenance & Evidence