反应详情

2-Amino-2-thioxoethyl pivalate (3.0 g, 17.12 mmol) and 3-bromo-2-oxopropanoic acid (3.14 g, 18.83 mmol) were dissolved in EtOH (20 mL), 4 Å molecular sieves added and the reaction mixture heated at reflux for 20 h then cooled to RT, filtered, washed with EtOH and evaporated in vacuo. The residual semi solid was treated with 50% EtOAc/DCM and the resulting light brown solid filtered off. The filtrate was evaporated in vacuo and the residue purified by chromatography on silica with 20% EtOAc/isohexane as eluent to afford the sub-title compound as a pale yellow oil. Yield: 2.47 g

1. addition4 Å molecular sieves added
2. temperaturethe reaction mixture heated
3. temperatureat reflux for 20 h
4. filtrationfiltered
5. washwashed with EtOH
6. customevaporated in vacuo
7. additionThe residual semi solid was treated with 50% EtOAc/DCM
8. filtrationthe resulting light brown solid filtered off
9. customThe filtrate was evaporated in vacuo
10. customthe residue purified by chromatography on silica with 20% EtOAc/isohexane as eluent