反应 #41991

ord-71866f818b4e40e097b0c842d5917d59

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    洗涤wash with 1N aqueous hydrochloric acid (2×)
  2. 2
    干燥dry over anhydrous sodium sulfate
  3. 3
    过滤filter
  4. 4
    浓缩concentrate solution in vacuo
  5. 5
    其他Purify the residue on silica eluting with 0 to 75% ethyl acetate/hexanes over 30 minutes

实验过程

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).

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US07728150B2uspto-grants-2010_06