반응 #643124

ord-92475f5a0b8d4fc596ef2cd682ddf001

반응 조건

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

후처리

  1. 1
    온도after cooling
  2. 2
    기타the solvent was evaporated
  3. 3
    workup.DISSOLUTIONThe crude material was dissolved in dichloromethane (100 mL)
  4. 4
    여과filtered through a short plug of silica gel, which
  5. 5
    세척was washed with another bolus of dichloromethane (100 mL)
  6. 6
    기타The organic eluent was evaporated

실험 절차

A flask was charged with 5-amino-1-methyl-1H-indole (8.8 g; 60 mmol), thiocarbonyl diimidazole (10.7 g; 60 mmol) and ethyl acetate (200 mL). The reaction was heated at 50° C. for five minutes, and after cooling, the solvent was evaporated. The crude material was dissolved in dichloromethane (100 mL) and filtered through a short plug of silica gel, which was washed with another bolus of dichloromethane (100 mL). The organic eluent was evaporated to give 5-isothiocyanato-1-methyl-1H-indole (8.9 g; 47 mmol).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US08053456B2uspto-grants-2011_11