반응 #161710

ord-85f255f912d74627b1b16b998fbcf446

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도while being cooled
  2. 2
    workup.WAITfor a further 1 h at RT
  3. 3
    workup.STIRRINGthe mixture was stirred for 10 min
  4. 4
    기타The organic phase was separated off
  5. 5
    세척washed with water (1×30 mL) and 1M hydrochloric acid (1×50 mL)
  6. 6
    기타dried on sodium sulphate
  7. 7
    여과filtered
  8. 8
    기타evaporated down i
  9. 9
    기타The product was reacted further without any further purification

실험 절차

1.04 g (5.50 mmol) benzyl-(2,2,2-trifluorethyl)-amine and 5.50 mL (5.50 mmol) of a 1M sodium hydroxide solution were added dropwise while cooling with a bath of ice/ethanol to 1.00 g (5.65 mmol) 6-chloropyrimidine-4-carboxylic acid chloride in 20 mL dichloromethane. The mixture was first stirred for 2 h while being cooled and then for a further 1 h at RT. 50 mL of a saturated sodium hydrogen carbonate solution were added and the mixture was stirred for 10 min. The organic phase was separated off, washed with water (1×30 mL) and 1M hydrochloric acid (1×50 mL), dried on sodium sulphate, filtered and evaporated down i. vac. The product was reacted further without any further purification.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US08829006B2uspto-grants-2014_09