反应详情

To a stirring solution of 3-amino-6-chloro-5-trifluoromethyl-pyrazine-2-carboxylic acid ethyl ester (Intermediate 7A) (165 mg, 0.612 mmol) in dry ethanol (10 ml), 2M NaOH (0.306 ml, 0.612 mmol) was added. After stirring at RT for 10 minutes, the reaction mixture was poured into water (30 ml) and the pH taken to 6 with the addition of 1M HCl. The product was extracted with EtOAc (2×30 ml). The organics were combined and washed with brine (20 ml), dried (MgSO4) and concentrated in vacuo. The crude material was purified by preparative LC-MS using 0.1% TFA/MeCN/Water system to afford the title compound. MS m/z 244 [M+H]+

1. extractionThe product was extracted with EtOAc (2×30 ml)
2. washwashed with brine (20 ml)
3. dry with materialdried (MgSO4)
4. concentrationconcentrated in vacuo
5. customThe crude material was purified by preparative LC-MS