反应详情

6-Chloro-5-(4-chloro-phenyl)-nicotinic acid methyl ester (30.9 g, 0.11 mol) was dissolved in a mixture of tetrahydrofuran (750 mL) and water (250 mL). Lithiumhydroxid monohydrate (13.8 g, 0.33 mol) was added and the mixture was stirred and heated at reflux-temperature for 1 h. After cooling to room temperature the mixture was acidified with hydrochloric acid (2N, 240 mL) and extracted with methyl-t-butylether. Organic phases were pooled, dried with MgSO4 and the mixture concentrated in vacuo. The title compound crystallized from the concentrated solution as a white solid (quant.); MS (ISP) 266.0 (M−H)

1. temperatureheated
2. temperatureat reflux-temperature for 1 h
3. extractionextracted with methyl-t-butylether
4. dry with materialdried with MgSO4
5. concentrationthe mixture concentrated in vacuo
6. customThe title compound crystallized from the concentrated solution as a white solid (quant.)