Sodium Bicarbonate → HCID 67218105, compound

Participants

Reaction Steps

A solution of ethyl chlorooximidoacetate (9.0 g, 59.1 mmol) in ethylacetate (30 ml) was added at ambient temperature with a syringe pump over a period of 40 h to a suspension of 1,3-dichloro-5-(3,3,3-trifluoroprop-1-en-2-yl)benzene (prepared according to WO 2005/085216) (9.5 g, 39.4 mmol) and sodium hydrogen carbonate (15.9 g, 189 mmol) in ethylacetate (85 ml). The reaction mixture was diluted with ethylacetate and washed with water. The organic phase was separated dried over sodium sulfate and concentrated. The residue was purified by chromatography over silica (cyclohexane/ethylacetate; 4/1) to give 8.9 of a yellow oil. 1H-NMR (CDCl3, 400 MHz): 7.45 (m, 3H), 4.49 (q, 2H), 3.96 (d, 1H), 3.59 (d, 1H), 1.40 (t, 3H).

Provenance & Evidence