Step 8 : 3 - [ 1 -(2,4-Dichlorobenzyl)-6-trifluoromethyl- 1 H-indazol-3 -yl] -acrylic acid ethyl ester.
1 -(2,4-Dichlorobenzyl)-6-trifluoromethyl- 1 H-indazole-3 -carbaldehyde (2.0 g, 0.00536 mol) was dissolved in CH2Cl2 (50 mL) and Wittig reagent (carbethoxymethylene) triphenylphosphorane (1.06 g, 0.0536 mol) was added to the solution. The homogeneous reaction mixture was heated to reflux in an oil bath for 12 h. The reaction progress was monitored by TLC. The reaction mixture was cooled to room temperature and worked up by quenching into water and separating the organic layer. Removal of the CH2Cl2 yielded the crude product, which was purified by column chromatography to yield the pure product (2.25 g, 95%) as a white solid, mp 186-188 0C.
1H NMR (CDCl3) 8.08 (d, J = 8.5 Hz, 1 H), 7.99 (d, J = 16.2 Hz, 1 H), 7.74 (s, 1 H), 7.52 (d, J = 8.5 Hz, 1 H), 7.47 (d, J = 2.0 Hz, 1 H), 7.16 (dd, J = 8.3 and 2.0 Hz, 1 H), 6.84 (d, J = 8.3 Hz, 1 H), 6.82 (d, J = 16.2 Hz, 1 H), 5.72 (s, 2 H), 4.32 (q, J = 7.1 Hz, 2 H), 1.38 (t, J = 7.1 Hz, 3 H).
MS (FAB) m/z: 443 (M+ + 1).
see
https://www.google.im/patents/WO2011005759A2?cl=en
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