反应详情

温度

90 °C

Lithium hydroxide (2 N, 2 ml) was warmed to 40° C. and a solution of ethyl 4-cyano-5-methyl-1H-pyrrole-2-carboxylate (Intermediate 14, 0.16 g) in 2 ml of MeOH was added. The reaction temperature was gradually increased to 90° C. and the reaction was stirred at that temperature for 2 hours. Then MeOH was removed and the remaining aqueous solution was cooled to 0° C. and acidified with 3 M HCl (pH ˜2). The acidic solution was extracted with EtOAc, the combined organic extracts were dried over magnesium sulfate and concentrated to give brown solid (0.07 g, crude).

1. customThen MeOH was removed
2. temperaturethe remaining aqueous solution was cooled to 0° C.
3. extractionThe acidic solution was extracted with EtOAc
4. dry with materialthe combined organic extracts were dried over magnesium sulfate
5. concentrationconcentrated
6. customto give brown solid (0.07 g, crude)