反应 #67579

ord-28a4d71b5ba24896aa0d31b613757e0e

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    其他fitted with a water condenser
  2. 2
    workup.WAITAfter a few minutes an exotherm was observed
  3. 3
    其他After 16 h the excess methylhydrazine was removed under reduced pressure
  4. 4
    萃取the resulting solution was extracted with ether (6×100 ml)
  5. 5
    干燥The combined extracts were dried (K2CO3)
  6. 6
    浓缩concentrated

实验过程

2-Chloropyrazine (1 g, 8.3 mmol) and methylhydrazine (1.31 mL, 25 mmol) were mixed together in a flask fitted with a water condenser. After a few minutes an exotherm was observed. After 16 h 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 a light orange solid 370 mg of N-Methyl-N-pyrazin-2-yl-hydrazine.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US08524764B2uspto-grants-2013_09