Dichloromethane → HCID 18696594, compound

Participants

Reaction Steps

Triphosgene (40.1 g) was added to a solution of crude title compound of Step C (15.4 g) in methylene chloride (550 mL) at 0° C. The mixture was heated at reflux for 4 h, cooled to room temperature and stirred overnight. The reaction mixture was concentrated to a brown oil which was dissolved in methylene chloride, washed with water and the aqueous layer extracted three times with methylene chloride. The combined organic extracts were dried (MgSO4), filtered and concentrated to a brown oil. Purification by flash chromatography (1:1 hexane:ethyl acetate) provided 5.34 g of the title compound of Step D as a yellow solid melting at 129-130° C. 1H NMR (CDCl3): δ 8.10 (d,1H), 7.72 (d,1H), 3.80 (s,3H), 3.52 (s,3H).

Provenance & Evidence