Ethanol → HCID 178457732, compound

Participants

Reaction Conditions

Reaction Steps

The product of Intermediate 10 (8.00 g, 38.8 mmol) was combined with CDI (7.24 g, 44.6 mmol) and DMF (80 mL). The reaction was aged at 105° C. for 45 min and cooled to about 77° C. Cumyl amine (7.26 mL, 50.4 mmol) and NEt3 (5.41 mL, 38.8 mmol) were added and the reaction continued to age at 77° C. for an additional 5 h. The reaction was concentrated and then diluted with CH2Cl2 and washed with aq. HCl (2 M) and water. The organic portion was concentrated and suspended in Et2O (270 mL) and aged for 1 h 40 min before the product was isolated by filtration. The solid was then suspended in 10% EtOH/90% Et2O (200 mL) and aged about 16 hrs before it was isolated by filtration and dried to afford the title compound. HPLC/MS: 342.1 (M+1); Rt=2.66 min.

Provenance & Evidence