반응 #312186

ord-3408868038b944e5b7875bb103e42040

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타After the reaction
  2. 2
    세척the reaction product was washed with water, with a sodium bicarbonate aqueous solution, with a saturated sodium thiosulfate solution
  3. 3
    건조with water and dried over anhydrous sodium sulfate
  4. 4
    workup.DISTILLATIONChloroform was distilled off under a reduced pressure
  5. 5
    세척the resulting crystals were washed with hexane
  6. 6
    기타dried

실험 절차

In 150 ml of chloroform, 5.5 g of 2-(3-hydroxyphenoxy)-3-chloro-5-trifluoromethyl pyridine was dissolved and then, 3.5 g of bromine was added dropwise to the solution at a temperature of 10° to 15° C. After the reaction, the reaction product was washed with water, with a sodium bicarbonate aqueous solution, with a saturated sodium thiosulfate solution and then, with water and dried over anhydrous sodium sulfate. Chloroform was distilled off under a reduced pressure and the resulting crystals were washed with hexane and dried to obtain 3.0 g of 2-(3-hydroxy-4-bromophenoxy)-3-chloro-5-trifluoromethyl pyridine having a melting point of 124° to 127° C.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US04235621uspto-grants-1980_11