반응 #613873

ord-704d58b3692d40f9bf7d48c6d281792a

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    농축The reaction mixture was concentrated under reduced pressure
  2. 2
    추출the aqueous layer was extracted with dichloromethane
  3. 3
    건조The combined organic phases were dried over MgSO4
  4. 4
    기타the solvents were removed under reduced pressure
  5. 5
    기타isolated crude product
  6. 6
    기타was used in the next reaction step

실험 절차

A solution of 1.6 g of 5-(4-Chloro-phenyl)-2-methyl-6-(4-trifluoromethyl-phenyl)-nicotinic acid ethyl ester and 136 mg of LiOH in 5 ml of THF and 5 ml of water was stirred at room temperature for 16 h. After 16 h, the mixture was brought to pH 2 by addition of 1 M hydrochloric acid. The reaction mixture was concentrated under reduced pressure and the aqueous layer was extracted with dichloromethane. The combined organic phases were dried over MgSO4 and the solvents were removed under reduced pressure. The residue was codistilled twice with dichloromethane and twice with toluene The isolated crude product was used in the next reaction step. Yield: 1.6 g.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US09346757B2uspto-grants-2016_05