Ammonium Acetate → HCID 15346450, compound

Participants

Reaction Steps

22.4 g (0.1 mol) of 2-(4-methylphenyl)-1,3-dithian-5-one and 77.1 g (1.0 mol) of ammonium acetate were stirred in 250 ml of methanol with the addition of 37.5 g of molecular sieve (3 Å) for 30 minutes and 6.30 g (0.1 mol) of sodium cyanoborohydride were then added in portions at 20° C. The mixture was stirred at room temperature for 48 hours, diluted with methanol and filtered. The filtrate was concentrated and the residue was taken up in dilute hydrochloric acid/toluene. The hydrochloric acid phase was rendered basic with concentrated sodium hydroxide solution and extracted with ether. This gave 2.2 g of product as a colorless oil (9.8% of theory), which was reacted without further purification.

Provenance & Evidence