反応 #663114

ord-69ba2380c54f46a6a53d84b16db946d8

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    その他The volatiles were removed in vacuo
  2. 2
    その他The crude product was purified on silica

実験手順

A solution of [1-(5-Bromo-2-hydroxy-benzyl)-5-methyl-1H-pyrazol-4-yl]-acetic acid ethyl ester, 2, (0.18 g g 0.51 mmol), triphenylphosphine (0.26 g, 1.02 mmol), di-tert-butylazodicarboxylate (0.23 g, 1.02 mmol) and 2-ethylbutan-1-ol (0.116 ml, 1.02 mmol) in a mixture of THF (1 mL) and toluene (2 ml) was at 120° C. on microwave for 20 min. The volatiles were removed in vacuo. The crude product was purified on silica to yield {1-[5-bromo-2-(2-ethyl-butoxy)-benzyl]-5-methyl-1H-pyrazol-4-yl}-acetic acid ethyl ester, 3.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US09035071B2uspto-grants-2015_05