반응 #1286637

ord-4409e63ab65b4efba1578743707adfc3

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    추출extracted with ethyl acetate (3 times)
  2. 2
    세척The combined extracts were washed with water (4 times)
  3. 3
    건조dried (anhydrous sodium sulphate)
  4. 4
    기타evaporated
  5. 5
    기타to yield a brown solid, which
  6. 6
    기타was triturated with ether
  7. 7
    여과filtered

실험 절차

The compound from step (a) above (24.2 mmol), N,N-dimethylaminothiocarbamoyl chloride (37 mmol) in dimethyl formamide (250 ml) were stirred rapidly in the presence of potassium carbonate (60 mmol) for 24 hours, adding more potassium carbonate (1 g) after 18 hours. The mixture was acidified (to pH4) with dilute hydrochloric acid and extracted with ethyl acetate (3 times). The combined extracts were washed with water (4 times), dried (anhydrous sodium sulphate) and evaporated to yield a brown solid, which was triturated with ether, and filtered to give the sub-title compound.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US04900751uspto-grants-1990_02