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With dicyclohexyl-carbodiimide In dichloromethane at 20℃;
Ethyl 2-chloropyrimidine-4-carboxylate (9.B). The reaction mixture of2-chloropyrimidine-4-carboxylic acid, 9.A (avialable from Anichem LLC, 1.00 g, 6.3 mmol), l^-dicyclohexylcarbodiimide (1.4 g, 6.9 mmol) and ethanol (0.32 g, 6.9 mmol) in DCM (10 ml) was stirred at room temperature overnight. The solid was filtrated off. DCM (80 ml) was added and washed with brine (30 ml) and dried over MgSO4. The solvent was evaporated. The crude product was purified by Cobi-Flash silica gel column to give 9.B. 0.74 g, yield, 63percent. 1H NMR (400 MHz, chloroform-;/) δ ppm 8.87 (1 H, d, J= 4.7 Hz), 7.95 (1 H, d, J = 4.7 Hz), 4.51 (2 H, q, J = 7.4 Hz), 1.45 (3 H, t, J = 7.0 Hz). MS ESI (pos.) m/e: 187.0 (M+H)+.
50%
With dmap; dicyclohexyl-carbodiimide In dichloromethane at 20℃; for 24 h;
[616] Step A: 2-chloropyrimidine-4-carboxylic acid ethyl ester [617] After 2-chloropyrimidin-4-carboxylic acid (0.223 g, 1.4 mmol) was dissolvedin DCM (7 mL), dicyclohexylcarbodiimide (0.29 g, 1.4 mmol), DMAP (0.017 g, 0.14mmol) and EtOH (0.1 mL, 1.4 mmol) were added thereto, and the mixture wasstirred at room temperature for 24 hours. After the termination of thereaction, the reactant was filtered and separated by column chromatography toobtain the title compound (0.13 g, 50percent).
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