반응 #1528932

ord-43387abddb81485382b6e79ede2d9757

용매

반응 조건

온도
95°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도After cooling
  2. 2
    기타the mixture is evaporated to dryness under reduced pressure
  3. 3
    workup.ADDITIONThe resulting residue is treated with water
  4. 4
    여과The precipitate is filtered off
  5. 5
    추출the filtrate extracted twice with n-butanol
  6. 6
    기타The combined organic extracts are evaporated

실험 절차

A mixture consisting of 50 mL dioxane, 25 mL water and 18.75 mL 2M aqueous sodium hydroxide solution is added to 3-(4-methyl-1-piperazinyl)-5-(trifluoromethyl)-benzonitrile (2.69 g, 10 mmol) and the reaction mixture shaken for 16 hours at 95° C. After cooling, the mixture is evaporated to dryness under reduced pressure. The resulting residue is treated with water, the pH adjusted to ˜5-6 with 2M hydrochloric acid. The precipitate is filtered off and the filtrate extracted twice with n-butanol. The combined organic extracts are evaporated to yield the title compound as a solid.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US07655669B2uspto-grants-2010_02