Sulfuric Acid → HCID 71179236, compound

Participants

Reaction Conditions

Reaction Steps

H2SO4 (110 mL) was heated to 40° C. Compound 61 (7.6 g, 12.3 mmol) was added in portions. The reaction mixture was heated to 100° C., kept at this temperature for 2 h (TLC monitoring, CH2Cl2/ethyl acetate 4:1), and poured into ice. The formed gray precipitate was filtered off. Then CHCl3/MeOH 4:1 (500 mL) was poured into the filter. The solid on the filter dissolved, and the formed solution was transferred into a separation funnel. An aqueous solution of Na2CO3 was added. The organic layer was separated, dried with Na7SO4, and evaporated. Acetonitrile was added to the residue. A beige precipitate was filtered off, washed with acetonitrile, with ether, and dried to give 1.56 g (23%) of a beige crystalline product.

Provenance & Evidence