반응 #8185

ord-b83aba9157f44fd9b0f7974734e9190c

반응 조건

온도
60°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도the mixture is cooled to ambient temperature
  2. 2
    온도is warmed to 50° C
  3. 3
    기타The catalyst is removed by filtration
  4. 4
    세척the cake is rinsed with 50° C. tetrahydrofuran (4×50 mL)
  5. 5
    농축The filtrate is concentrated to a solid which
  6. 6
    기타is dried in a 50° C. vacuum oven

실험 절차

A mixture of 3-(2-methyl-2-nitropropyl)-7-(benzyloxy)indole (25.0 g, 77.1 mmol), Raney Nickel® (9.5 g wet lump), and 3A ethanol (250 mL) is pressurized to 50 psig with H2 and is heated to 60° C. After 1 hour, the mixture is cooled to ambient temperature. The mixture is diluted with tetrahydrofuran (100 mL) and is warmed to 50° C. The catalyst is removed by filtration and the cake is rinsed with 50° C. tetrahydrofuran (4×50 mL). The filtrate is concentrated to a solid which is dried in a 50° C. vacuum oven to provide 22.41 (99%) of 2-methyl-1-[7-(benzyloxy)indol-3-yl]prop-2-ylamine. MS (ES+) m/z 295 (100%).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US07087635B2uspto-grants-2006_08