反应详情

KOH (13g, 235 mmol) was added to a mixture of ethanol/water (100 mL/100 mL) containing nitrile 1-2 (12.4 g, 58.68 mmol) and refluxed for 8 hours. Ethanol was removed in vacuo and the residue was acidified to pH=2 with aqueous HCl. The precipitated solid was filtered, washed with water, and dried in a vacuum oven overnight. The recoverd 13.5 g of acid 1-3 was used in the following step with no further purification. NMR CDCl3 (δ): 7.97 (2H, m); 7.45 (3H, m); 2.84 (4H, m); 2.35 (3H, s). M+1=232.1

1. temperaturerefluxed for 8 hours
2. customEthanol was removed in vacuo
3. filtrationThe precipitated solid was filtered
4. washwashed with water
5. customdried in a vacuum oven overnight
6. customThe recoverd 13.5 g of acid 1-3 was used in the following step with no further purification