反应详情

温度

150 °C

A well stirred solution of 0.17 g (1.59 mmol) of 3-chloro-1H-[1,2,4]triazole in 1.0 ml of 1-methyl-pyrrolidin-2-one was treated at RT with 0.058 g (1.32 mmol) of a sodium hydride (55% in mineral oil). After 30 min, 0.20 g (0.44 mmol) of [6-chloro-3-methyl-5-(3-trifluoromethyl-phenyl)-pyridin-2-yl]-(4-pyrrolidin-1-yl-piperidin-1-yl)-methanone (example 3) was added and the reaction mixture was heated up to 150° C. After 24 hours, it was poured into crashed ice and extracted twice with EtOAc; 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 95:5) to give 0.11 g (48%) of the title compound as yellow oil. MS: 519.3 (MH+, 1Cl).

1. waitAfter 24 hours
2. additionit was poured
3. extractionextracted twice with EtOAc
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 95:5)