反应详情

To a 0° C. solution of 2-(2,6-dichloro-phenyl)-4-isopropyl-2H-pyrazole-3-carboxylic acid methyl ester (2.2 g, 6.8 mmol) in THF (30 mL) is added DIBAL-H (33.7 mL, 1M in toluene). The reaction mixture is stirred at ambient temperature overnight. The reaction is quenched by the addition of methanol and is concentrated under reduced pressure. The residue is partitioned between 5N NaOH and EtOAc. The layers are separated and the organic layer is filtered through a pad of diatomaceous earth. The filtrate is concentrated under reduced pressure to give the title compound as a light yellow solid, (1.6 g, 80%). 1H NMR (400 MHz, CDCl3): δ 7.67 (s, 1H), 7.44 (d, 2H), 7.34 (dd, 1H), 4.45 (s, 2H), 3.00 (m, 1H), 1.32 (d, 6H).

1. customThe reaction is quenched by the addition of methanol
2. concentrationis concentrated under reduced pressure
3. customThe residue is partitioned between 5N NaOH and EtOAc
4. customThe layers are separated
5. filtrationthe organic layer is filtered through a pad of diatomaceous earth
6. concentrationThe filtrate is concentrated under reduced pressure