Phosphorus oxychloride → HCID 87571378, compound

Participants

Reaction Steps

A mixture of EXAMPLE 80D (9.97 g, 39.5 mmol) and phosphoryl trichloride (110 ml, 1184 mmol) was stirred at 80° C. for 5 hours. The mixture was cooled to room temperature, then concentrated to dryness. Water (150 mL) was added cautiously. The mixture was cooled with an ice bath and adjusted to pH˜11 with concentrated aqueous NaOH, then stirred for 30 minutes. The solid was collected by filtration, washed with water (3×50 mL), and dried in a vacuum oven overnight at ˜50° C. to provide the title compound. (ESI(+)) m/e 271.1 (M+H)+.

Provenance & Evidence