反应详情

温度

82.5 °C

A mixture of methyl 2-bromo-1,3-thiazole-5-carboxylate (3 g, 13.5 mmol), 3-pyrrolidinol (1.3 g, 14.9 mmol) and DBU (4.1 mL, 27 mmol) in dioxane (50 mL) was heated at 80-85° C. overnight. After cooling, the mixture was diluted with water and extracted five times with EtOAc. The combined EtOAc extracts were washed with water, dried (Na2SO4) and concentrated to give the crude title compound as a light brown solid. 1H NMR (400 MHz, acetone-d6): δ 7.83 (s, 1H), 4.65 (m, 1 H), 4.33 (m, 1 H), 3.79 (s, 3 H), 3.67-3.45 (m, 4 H), 2.29-2.19 (m, 1 H), 2.11 (m, 1 H).

1. temperatureAfter cooling
2. extractionextracted five times with EtOAc
3. washThe combined EtOAc extracts were washed with water
4. dry with materialdried (Na2SO4)
5. concentrationconcentrated