反応 #5443

ord-fb02e62a59a44836a806f3943ed12dcc

反応条件

温度
-78°CELSIUS
詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    温度The reaction was warmed to 0° C. for 4 h
  2. 2
    温度cooled to -78° C
  3. 3
    その他The reaction was quenched by the addition of 5 ml methanol
  4. 4
    その他the solvent was evaporated
  5. 5
    その他The resulting solid was recrystallized from ethanol and ether

実験手順

The product from Example 9 (0.490 g) was dissolved in 25 ml methylene chloride and cooled to -78° C. To the reaction was added 0.69 ml BBr3. The reaction was warmed to 0° C. for 4 h and then cooled to -78° C. The reaction was quenched by the addition of 5 ml methanol and the solvent was evaporated. The resulting solid was recrystallized from ethanol and ether to yield 0.470 g white solid, mp: 187°-9° C. NMR (d6DMSO) δ0.88 (t, 3H), 1.65 (m, 2H), 2.60-4.10 (m, 10H), 6.65 (d, 1H), 6.70 (d, 1H), 7.05 (t, 1H).

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US05244888uspto-grants-1993_09