Toluene → HCID 14446267, compound

Participants

Reaction Conditions

Reaction Steps

The starting material 1,2,6,7,8,8a-hexahydro-3,6,6,8a-tetramethyl-4-acenaphthylenecarbaldehyde is prepared by substantially following the procedures of Fehr et al., U.S. Pat. No. 5,162,588. Specifically, in a 2.5 liter flask equipped with a mechanical stirrer, a condenser, a thermometer and a nitrogen inlet, α-chloro-o-xylene (available from Fluka Chemical Corp., Ronkonkoma, N.Y., 140.6 g) is mixed with ethyl acetoacetate (130 g), a fine powder of potassium carbonate (414 g) and 800 ml of toluene. The mixture is heated to 100° C. for 20 h. After cooling, H2O is added (500 ml). The organic phase is washed with water and saturated NaCl, then dried over Na2SO4 and evaporated, resulting in a brown oil. The oil is distilled (120° C.-125° C./5.65 Pa) to yield ethyl-2-acetyl-3-(2-methyl-1-phenyl)propanoate.

Provenance & Evidence