Реакция #41991

ord-71866f818b4e40e097b0c842d5917d59

Растворители

Условия реакции

Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    Промывкаwash with 1N aqueous hydrochloric acid (2×)
  2. 2
    Сушкаdry over anhydrous sodium sulfate
  3. 3
    Фильтрацияfilter
  4. 4
    Концентрированиеconcentrate solution in vacuo
  5. 5
    ДругоеPurify the residue on silica eluting with 0 to 75% ethyl acetate/hexanes over 30 minutes

Методика

Dissolve 3-(1-ethyl-5-fluoro-indan-1-yl)-1H-indol-7-ylamine (0.35 g, 1.19 mmol) in pyridine (3 ml). Add methyl chloroformate (0.10 ml, 1.31 mmol, 1.1 equivalents) and stir at room temperature under nitrogen overnight. Dilute with ether, wash with 1N aqueous hydrochloric acid (2×), dry over anhydrous sodium sulfate, filter, and concentrate solution in vacuo. Purify the residue on silica eluting with 0 to 75% ethyl acetate/hexanes over 30 minutes to provide the title compound as a white solid (0.15 g, 36%). LC-MS m/z 353.1 (M++1).

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US07728150B2uspto-grants-2010_06