反应详情

Ethyl chloroformate (1.3 mL; 13.5 mmol) is added dropwise to a solution of methyl N-({2-amino-5-[(1-bromo-2-methylindolizin-3-yl)carbonyl]phenyl}carbonyl)glycinate (2 g; 4.5 mmol) in 9 mL of pyridine at 0° C. After 15 min of stirring at ambient temperature, the reaction medium is concentrated to dryness and then diluted with ethyl acetate. The solution is washed with a 0.1 M hydrochloric acid solution and a saturated solution of sodium chloride, dried over sodium sulphate and concentrated to dryness. The yellow solid obtained is dissolved in 20 mL of anhydrous tetrahydrofuran and heated at reflux in the presence of diaza(1,3)bicyclo[5,4,0]undec-7-ene (1.35 mL; 9 mmol) for 1 h. The reaction medium is diluted with ethyl acetate, washed with a 0.1 M hydrochloric acid solution and a saturated solution of sodium chloride, dried over sodium sulphate and concentrated to dryness to give 2 g (95%) of a yellow powder.

1. concentrationthe reaction medium is concentrated to dryness
2. additiondiluted with ethyl acetate
3. washThe solution is washed with a 0.1 M hydrochloric acid solution
4. dry with materiala saturated solution of sodium chloride, dried over sodium sulphate
5. concentrationconcentrated to dryness
6. customThe yellow solid obtained
7. temperatureheated
8. washwashed with a 0.1 M hydrochloric acid solution
9. dry with materiala saturated solution of sodium chloride, dried over sodium sulphate
10. concentrationconcentrated to dryness