반응 #67582

ord-facf30b996f1484aaf341a84a6141e83

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타fitted with a water condenser
  2. 2
    온도to reflux
  3. 3
    기타the excess methylhydrazine was removed under reduced pressure
  4. 4
    추출the resulting solution was extracted with ether (6×100 ml)
  5. 5
    건조The combined extracts were dried (K2CO3)
  6. 6
    농축concentrated

실험 절차

3,6-Dichloro-pyridazine (1 g, 6/5 mmol) was placed in a flask fitted with a water condenser and methylhydrazine (1.31 mL, 25 mmol) was added dropwise. An immediate exotherm was observed and methylhydrazine begins to reflux. When the reaction had subsided, the mixture was left for 16 hours, and the excess methylhydrazine was removed under reduced pressure. The cooled residue was stirred with aqueous sodium hydroxide solution (20 ml of 20%), and the resulting solution was extracted with ether (6×100 ml). The combined extracts were dried (K2CO3) and concentrated to give 427 mg of N-(6-Chloro-pyridazin-3-yl)-N-methyl-hydrazine.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US08524764B2uspto-grants-2013_09