反应详情

Sodium (4.6 g, 200 mmol) was added to EtOH (500 mL) and the mixture was stirred until a clear solution was obtained. Then, step B product, 2-c, (20.1 g, 100 mmol) and diethyl 2-(ethoxymethylene)malonate (21.6 g, 100 mmol) were added to the clear mixture, respectively. The reaction mixture was refluxed overnight and then concentrated under vacuum, washed with EA. The wet cake was then dried to afford compound 2-d (40.0 g, crude). LC-MS: (M+H)+ 289. The crude was directly used to next step without further purification.

1. customwas obtained
2. temperatureThe reaction mixture was refluxed overnight
3. concentrationconcentrated under vacuum
4. washwashed with EA
5. customThe wet cake was then dried
6. customto afford compound 2-d (40.0 g, crude)
7. customThe crude was directly used to next step without further purification