反応 #1972323

ord-1e44904c37394059ab0a9681c4bcfcac

溶媒

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    温度It was heated
  2. 2
    温度at reflux for 3 hours
  3. 3
    温度the mixture was cooled
  4. 4
    その他the solvent was removed under reduced pressure
  5. 5
    その他to give a yellow solid

実験手順

Triethylphosphite-carbomethoxyborane (4) (1.13 g, 4.75 mmol) and Me3SiI 2.70 ml, 18.97 mmol) were taken in anhydrous CH3CN (45 ml) under nitrogen atmosphere. Immediately, the mixture became brown. It was heated at reflux for 3 hours. During this time, the brown color completely disappeared, the mixture was cooled, and the solvent was removed under reduced pressure to give a yellow solid. 11B NMR CDCl3):δ=15 ppm, br. s., 0.2 ppm, br. s., major and a multiplet at -39 ppm, very small amount.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US05143907uspto-grants-1992_09