反应详情

4-Phenoxythiophenol (7.4 g, 36.3 mmol), 4-carboxymethylene-N-CBZ-piperidine (10 g, 36.3 mmol) and piperidine (1.8 ml, 36.3 mmol) were stirred overnight at 100-110° C. in a sealed flask. After cooling, the crude reaction mixture was partitioned between ethyl acetate and 1N hydrochloric acid, the organic layer was washed with brine, dried over magnesium sulfate, filtered, and concentrated in vacuo to give a yellow solid. The solid was triturated in 1:1 (v/v) ethyl ether/hexane (500 ml) to give 2-[4-(4-phenoxyphenylthio)-N-CBZ-piperidin-4-yl]-acetic acid as a white solid.

1. temperatureAfter cooling
2. customthe crude reaction mixture
3. customwas partitioned between ethyl acetate and 1N hydrochloric acid
4. washthe organic layer was washed with brine
5. dry with materialdried over magnesium sulfate
6. filtrationfiltered
7. concentrationconcentrated in vacuo
8. customto give a yellow solid
9. customThe solid was triturated in 1:1 (v/v) ethyl ether/hexane (500 ml)