반응 #645249

ord-f392fc23c3624e0bbbb713a5ea5747e4

반응 조건

온도
50°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도The mixture is cooled
  2. 2
    추출The mixture is extracted 3 times with in each case 150 ml of ethyl acetate
  3. 3
    건조the extracts are dried with sodium sulphate
  4. 4
    농축concentrated
  5. 5
    기타a rotary evaporator

실험 절차

9 g (40.9 mmol) of methyl 3,5-dichloro-2-aminobenzoate and 6.3 g (81.8 mmol) of 2-(aminooxy)ethanol are initially charged in 90 ml of methanol, and 22.1 g (122.7 mmol) of sodium methoxide as a 30% strength solution in methanol are added dropwise at 20° C. The mixture is stirred at 50° C. overnight. The mixture is cooled and poured onto 400 ml of water, and the pH is adjusted to 3 using 1 N hydrochloric acid. The mixture is extracted 3 times with in each case 150 ml of ethyl acetate and the extracts are dried with sodium sulphate and concentrated using a rotary evaporator.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US08062995B2uspto-grants-2011_11