反应详情

温度

140 °C

A mixture of commercially available 2-chloro-3-trifluoromethylpyridine (64.83 g, 357 mmol), 4-methoxybenzylamine (56 mL, 429 mmol) and DIPEA (73.4 mL, 429 mmol) in n-butanol (100 mL) was refluxed (oilbathtemp. 140° C.) for 3.5 days. Concentrated in vacuum, partitioned between 25% HCl and TBME, reextracted the organic layer twice with 25% HCl, the aqueous layer was made alkaline with 32% NaOH, extracted with TBME, washed with brine and dried over Na2SO4. Removal of the solvent in vacuum left a brown oil (105.21 g,>100%). Vacuum distillation gave the product as a colorless liquid (83.766 g, 83%, bp 139-141° C. at 1.4 mbar). MS (ISP) 283.1 [(M+H)+].

1. concentrationConcentrated in vacuum
2. custompartitioned between 25% HCl and TBME
3. extractionextracted with TBME
4. washwashed with brine
5. dry with materialdried over Na2SO4
6. customRemoval of the solvent in vacuum
7. waitleft a brown oil (105.21 g,>100%)
8. distillationVacuum distillation