反应详情

A mixture of 7-hydroxy-2-phenyl-4-trimethylsilanylethynyl-thiazolo[4,5-c]pyridine-6 carboxylic acid ethyl ester (113 mg, 0.28 mmole) and glycine (750 mg, 9.99 mmole) in 0.5 M sodium methoxide/methanol (20 ml) was refluxed for 3 days before it was cooled to room temperature and concentrated in vacuo. The residue was dissolved in water (30 ml) and extracted with dichloromethane (2×40 ml). The remaining aqueous layer was acidified to pH=2 with 1N HCl. The suspension was extracted with ethyl acetate (2×40 ml), washed with brine, dried over anhydrous sodium sulfate and concentrated in vacuo to give the title compound as a yellow solid (96 mg). MS: (+) m/z 354.20 (M+1), (−) m/z 352.16 (M−1).

1. temperaturewas refluxed for 3 days before it
2. concentrationconcentrated in vacuo
3. dissolutionThe residue was dissolved in water (30 ml)
4. extractionextracted with dichloromethane (2×40 ml)
5. extractionThe suspension was extracted with ethyl acetate (2×40 ml)
6. washwashed with brine
7. dry with materialdried over anhydrous sodium sulfate
8. concentrationconcentrated in vacuo