反应详情

Added sodium hydride (19 mg; 0.8 mmol) to a stirred suspension of 4H-Chromeno[4,3-d]thiazol-2-ylamine hydroiodide 19 (90 mg; 0.27 mmol) in dry tetrahydrofuran under nitrogen at room temperature. After 15 minutes, isonicotinoyl chloride hydrochloride (62 mg; 0.35 mmol) was added and the mixture allowed to stir for 3 hr. at room temperature and then concentrated in vacuo. The residue was diluted with water and extracted with ethyl acetate. The extracts were dried (sodium sulfate), filtered and concentrated in vacuo. Purification using reverse phase HPLC (eluent: acetonitrile/water/0.1% trifluoroacetic acid) provided 12 mg of N-(4H-Chromeno[4,3-d]thiazol-2-yl)-isonicotinamide 20 as the trifluoroacetate salt. ES-HRMS m/e calcd for C16H11N3OS (M+H) 310.0645, found 310.0646.

1. concentrationat room temperature and then concentrated in vacuo
2. additionThe residue was diluted with water
3. extractionextracted with ethyl acetate
4. dry with materialThe extracts were dried (sodium sulfate)
5. filtrationfiltered
6. concentrationconcentrated in vacuo
7. customPurification