반응 #8300

ord-6e9f813cdbf440e28165af869bd6f9f1

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도a gentle reflux throughout the addition
  2. 2
    기타The layers are separated
  3. 3
    세척the organic layer washed with brine
  4. 4
    건조dried (sodium sulfate)
  5. 5
    여과filtered
  6. 6
    농축concentrated in vacuo

실험 절차

4-Chlorobutyryl chloride (57 mL, 510 mmol) is added to a solution of benzophenone hydrazone (100 g, 510 mmol) and pyridine (41 mL, 510 mmol) in anhydrous dichloromethane (520 mL) under nitrogen at a rate that maintains a gentle reflux throughout the addition. The mixture is stirred for 0.5 h and poured into water (1 L). The layers are separated and the organic layer washed with brine, dried (sodium sulfate), filtered, and concentrated in vacuo to yield 4-chloro-butyric acid benzhydrylidene-hydrazide as a residue.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US07087626B2uspto-grants-2006_08