Acetic Anhydride → HCID 350142, compound

Participants

Reaction Steps

2-Amino-5-nitro-phenol (46) (20 g, 97.3 mmol) was suspended in THF (125 mL) and Acetic-anhydride (75 mL) was added. Di-methyl-amino-pyridine (DMAP) (300 mg, 2.45 mmol) was added and the mixture was stirred for 16 h at room temperature. A solid precipitated and was collected by filtration followed by rinsing with 3:1 hexane/EtOAc (3×100 mL). The solid was dried under high vacuum for 8 h to give the desired product (416) as a yellow powder (21 g, 88.2 mmol, 90.7% yield). LC-MS (ESI): (exact mass: 238.06) m/e=239.2 [M+1]+ (15%), 477.1 [2M+1]+ (100%).

Provenance & Evidence