Phosphorus oxychloride → HCID 91619162, compound

Participants

Reaction Conditions

Reaction Steps

To Intermediate 1A in THF (300 mL) was added TEA (33 mL, 238 mmol) and, after cooling to 0° C., POCl3 (7.3 mL, 79 mmol) was slowly added and the reaction was stirred at room temperature. After 24 h, the reaction was partitioned between EtOAc (200 mL) and aqueous NaHCO3 (100 mL). The aqueous layer was extracted with EtOAc (100 mL). The combined organic layers were washed with brine (50 mL) and dried (MgSO4). Purification by normal phase chromatography afforded 10.4 g (64.6%) of Intermediate 1 as a green solid. 1H NMR (400 MHz, CDCl3) δ 8.02 (d, J=8.59 Hz, 2H), 7.41 (d, J=8.34 Hz, 2H), 1.60 (s, 9H) ppm.

Provenance & Evidence