反应详情

温度

150 °C

A well stirred suspension of 0.30 g (0.66 mmol) of [6-chloro-3-methyl-5-(3-trifluoromethyl-phenyl)-pyridin-2-yl]-(4-pyrrolidin-1-yl-piperidin-1-yl)-methanone (example 3) and 0.098 g (2.0 mmol) of sodium cyanide in 5.0 ml of 1-methyl-pyrrolidin-2-one was heated for 16 hours at 150° C. After cooling down to RT, the reaction mixture was poured into crashed ice/NaCl-solution (sat. in H2O) and extracted three times with CH2Cl2; the organic phases were washed with water, dried over magnesium sulfate, filtered and evaporated. The residue was purified by flash column chromatography (CH2Cl2/MeOH 1:0 to 4:1) to give 0.086 g (29%) of 5-methyl-6-(4-pyrrolidin-1-yl-piperidine-1-carbonyl)-3-(3-trifluoromethyl-phenyl)-pyridine-2-carbonitrile as light yellow solid. MS: 443.4 (MH+); and 0.045 g (15%) of 5-methyl-6-(4-pyrrolidin-1-yl-piperidine-1-carbonyl)-3-(3-trifluoromethyl-phenyl)-pyridine-2-carboxylic acid amide as light yellow solid. MS: 461.4 (MH+).

1. temperatureAfter cooling down to RT
2. additionthe reaction mixture was poured
3. extractionextracted three times with CH2Cl2
4. washthe organic phases were washed with water
5. dry with materialdried over magnesium sulfate
6. filtrationfiltered
7. customevaporated
8. customThe residue was purified by flash column chromatography (CH2Cl2/MeOH 1:0 to 4:1)