Ethyl chloroformate → HCID 131722384, compound

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Reaction Steps

A solution of 2-methyl-(1,3,4,14b-tetrahydro-2H-dibenzo[b,f]pyrazino[1,2-d][1,4]oxazepine) (2.0 g, 7.5 mmol, prepared similarly as described in Neth. Appl. 6709520, Chem. Abs. 70, 115192 (1969)) in toluene (12 ml) was added drop wise to a stirred solution of ethyl chloroformate (1.26 g, 1.1 ml, 11.7 mmol) in toluene (8 ml) at 60° C. The mixture was heated at reflux temperature for 2 h. After cooling, the mixture was washed with a saturated solution of sodium bicarbonate (2×10 ml), water (10 ml), dried (MgSO4) and evaporated. The residue (2.5 g) was purified by column chromatography on silica gel (50 g) using benzene as eluent to give 1.95 g (80%) of 2-ethoxycarbonyl-(1,3,4,14b-tetrahydro-2H-dibenzo[b,f]pyrazino[1,2-d][1,4]oxazepine) as an oil.

Provenance & Evidence