Nitrogen → HCID 90685251, compound

Participants

Reaction Conditions

Reaction Steps

A reaction mixture of the mesylate of Step 7 (1.67 kg, 4.32 mol), DMF (8.35 L), NaN3 (0.457 kg, 7.03 mol) and Et3N (65 ml, 0.466 mol) under a constant stream of N2 was maintained between 66-70° C. After 18 h, the mixture was cooled to room temperature and H2O (8.45 L) was slowly added with vigorous stirring. The reaction mixture was filtered; the crystals were washed with 1:1 DMF:H2O (16 L), 3:7 DMF:H2O (8.5 L), and water (14 L). The dark brown solid was dried under vacuum and nitrogen.

Provenance & Evidence