Acetic Anhydride → HCID 14099335, compound

Participants

Reaction Steps

Compound (2) was prepared by the protocol already published [D2], but modified here. The modification was that sodium acetate was used [D3]. A mixture of sodium 6,8-dihydroxypyrene-1,3-disulfonate (1) (4.452 g, 10.16 mmol), sodium acetate (83.0 mg, 1.016 mmol) and acetic anhydride (5.8 mL) in DMF (250 mL) was stirred intensively at room temperature for 48 h with the exclusion of light. The reaction mixture was filtered through a Celite-kieselguhr bed (h=0.5 cm), and DMF was stripped off on a rotary evaporator at 50° C. and 0.1 Torr. The residue was recrystallized from an ethanol/water mixture (70 ml:10 ml), washed with acetone and dried in vacuo to give a yield of 4.242 g (83%) as yellow powder (melting point 245-247° C. (decomposition)).

Provenance & Evidence