反应详情

To 3,3,3-trifluoro-2-hydroxy-2-methylpropanoic acid (324 mg, 2.049 mmol) in NMP (5 ml) was added HATU (935 mg, 2.458 mmol) and DIPEA (1.073 ml, 6.15 mmol). After stirring for 5 minutes 3-amino-5-(trifluoromethyl)picolinohydrazide (Intermediate I) (451 mg, 2.049 mmol) was added and stirring continued at RT for 1 h. The reaction mixture was diluted with water and extracted with EtOAc. The combined organic extracts were washed with 1M HCl (100 ml), water (2×100 ml), brine and dried (phase separator) and concentrated in vacuo. Purification by chromatography on silica eluting with 0-30% EtOAc in iso-hexane afforded the title compound; 1H NMR 400 MHz, DMSO-d6: δ 10.3 (1H, s), 10.0 (1H, s), 8.0 (1H, s), 7.5 (1H, s), 7.1 (3H, s, overlap), 1.5 (3H, s). LC-MS Rt=0.98 min [M+H]+ 361.2 Method 2minLC_v003.

1. additionwas added
2. extractionextracted with EtOAc
3. washThe combined organic extracts were washed with 1M HCl (100 ml), water (2×100 ml), brine
4. customdried (phase separator)
5. concentrationconcentrated in vacuo
6. customPurification by chromatography on silica eluting with 0-30% EtOAc in iso-hexane