Dimethylformamide → HCID 178441001, compound

Participants

Reaction Conditions

Reaction Steps

A 500 ml. 3-neck, r.b. flask fitted with stirrer, condenser and thermometer was charged with the remainder of the filtrate from part A, the compound of Example I, C.(20.9 g. 0.0962 mole) and an additional 100 ml. dimethylformamide. The mixture was stirred overnight while heating at 110°C. The solution was chilled and the crystals were collected by filtration and dried at 60°C to yield 23 g. off white crystals, m.p. 260°- 268°C. The filtrate was concentrated to 150 ml. by rotary evapaorator and chilled. Crop II was collected and dried to yield 3.9 g. light yellow crystals, m.p. 238°-251°C. Both crops were dissolved in isopropanol (600 ml.) and filtered while hot. The filtrate was chilled and the crystals were collected and dried at 60°C to yield 13.2 g. light yellow crystals, m.p. 273°-276°C.

Provenance & Evidence