Acetic Acid → HCID 21516800, compound

Participants

Reaction Steps

A stirred mixture of 1α,1,2,3,4,4α-hexahydro- 6-methoxy-7,8-dichlorofluoren-9-one (8.3 g., 0.029 mole), 2,3-dichloro-5,6-dicyano-1,4-benzoquinone (20.5 g., 0.091 mole), benzene (300 ml.) and acetic acid (10 ml.) is heated at reflux under nitrogen for 64 hours. The reaction mixture is dissolved in a large volume of ethyl acetate (3 l.), the organic solution treated with sodium bisulfite solution, washed with water, 5% sodium hydroxide solution and water, separated, dried over magnesium sulfate and concentrated to give 1,2-dichloro-3-methoxyfluoren-9-one which after sublimation and trituration with acetonitrile give 3.9 g. melting at 268°-270°C.

Provenance & Evidence