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With sodium hydroxide; In ethanol; water; at 20℃; for 3h;
To a mixture of compound 14-4 (2.2 g, i2 mmol) in a mixed solvent of ethanol (10 mL) and water (5 mL) was added NaOH (1.9 g, 48 mmol). The mixture was stirred at rt for 3 hours. After the reaction was complete, the mixture was adjusted with hydrochloric acid (1 M) to pH 2 and concentrated in vacuo to remove ethanol. The mixture was diluted with water (50 mL). The resulting mixture was extracted with EtOAc (50 mL x 3). The combined organic layers were washed with saturated aqueous NaC1 solution, and dried over anhydrous Na2504 and concentrated in vacuo to give product 14-5 as a white solid (1.64 g, 88percent).
With sodium hydroxide; water; In 1,4-dioxane; at 50℃; for 3h;
<strong>[78208-72-7]5-isopropyl-1H-pyrazol-3-carboxylic acid ethyl ester</strong> (18.9 g, 104 mmol) and 1M NaOH solution (260 mL, 259 mmol) were dissolved in 1,4-dioxane (300 mL), the reaction was heated to 50° C. under nitrogen and stirred for 3 h. The reaction mixture was cooled, adjusted to pH 2 using concentrated hydrochloric acid and the solvent was removed under reduced pressure. The residual solid was azeotroped with toluene (2.x.30 mL), dissolved in ethyl acetate (500 mL) and washed with water. The aqueous phase was removed, extracted with ethyl acetate (2.x.200 mL) and the combined organic extracts were dried over MgSO4. The solvent was removed under reduced pressure and the residue was azeotroped with dichloromethane (2.x.50 mL) to give the title product (14.7 g) as a white solid; 1H NMR (400 MHz, DMSO-D6): delta 12.50-13.30 (bs, 2H), 6.42 (s, 1H), 2.84-2.94 (quin, 1H), 1.15-1.19 (d, 6H) ppm; LRMS (electrospray): m/z [M-H]+ 153.
Preparation 6 5-ISOPROPYL-1 H-PVRAZOLE-3-CARBOXYLIC acid ethyl ester 5-ISOPROPYL-1 H-PYRAZOLE-3-CARBOXYLIC acid (WO 03/035065, page. 485, example 17b) (1. 00G, 6. 49mmol) was dissolved in a mixture of concentrated sulphuric acid (1.5mL) and ethanol (25mL) and the reaction mixture heated at reflux for 3 hours. The reaction mixture was cooled, poured into water, basified with 0. 88 ammonia then extracted with ethyl acetate. The ethyl acetate was washed with brine, dried over magnesium sulphate and concentrated in vacuo to yield the title product, 514mg (43percent). 1HNMR (CDCI3, 400MHZ) : 1.30 (d, 6H), 1.38 (t, 3H), 3.64 (m, 1H), 4.38 (m, 2H), 6.63 (s, 1 H).
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