反应详情

1-(3-Dimethylaminopropyl)-3-ethyl-carbodiimide hydrochloride (434 mg, 2.26 mmol) was added to a stirred solution of 5-iodo-2-butoxynicotinic acid (615 mg, 1.92 mmol), 4-amino-3-ethyl-1-(2-methoxyethyl)-pyrazole-5-carboxamide (370 mg, 1.74 mmol), 1-hydroxybenzotriazole hydrate (346 mg, 2.26 mmol) and diisopropylethylamine (0.9 mL, 5.22 mmol) in tetrahydrofuran (12 mL) at room temperature under a nitrogen atmosphere. After 20 h the solvent was evaporated and the product was extracted from 10% sodium bicarbonate solution with dichloromethane (3×100 mL). The organics were dried (MgSO4) and concentrated to give a fawn solid. The solid was triturated with di-isopropylether to give an off-white solid (1.2 g).

1. customAfter 20 h the solvent was evaporated
2. extractionthe product was extracted from 10% sodium bicarbonate solution with dichloromethane (3×100 mL)
3. dry with materialThe organics were dried (MgSO4)
4. concentrationconcentrated
5. customto give a fawn solid
6. customThe solid was triturated with di-isopropylether