Dimethylformamide → HCID 88483256, compound

Participants

Reaction Conditions

Reaction Steps

The title A compound (9.29 g, 23.06 mmol) was added to a solution of the title E compound of Example 1 (8.34 g, 27.6 mmol) in dimethylformamide 115 mL) and cooled to 0° C. Hydroxybenzotriazole hydrate (3.87 g, 25.4 mmol), triethylamine (4.82 mL, 34.6 mmol) and 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide hydrochloride (4.86 g, 25.4 mmol) were added sequentially. After 16 hours at 25° C., a pH 4.01 buffer solution was added and the reaction mixture was stirred for an additional 10 minutes. The aqueous layer was extracted with ethyl acetate 2×500 mL) and the combined organic extracts were dried over sodium sulfate and concentrated. Purification of the crude product by flash chromatography yielded 9.37 g of the title B compound, which was characterized by MS and 13NMR.

Provenance & Evidence