反応 #80047

ord-25fbc025d0b046faa72ec4a436099d9c

溶媒

反応条件

温度
35°CELSIUS
詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    その他The reaction was quenched
  2. 2
    抽出The mixture was extracted with Et2O
  3. 3
    洗浄the combined organic layers were washed with H2O and saturated aqueous NaCl
  4. 4
    乾燥before being dried (MgSO4)
  5. 5
    濃縮concentrated under reduced pressure
  6. 6
    その他The title compound 613 mg (85%) was used without further purification

実験手順

To a solution of tert-butyl [1-(4-bromophenyl)-cyclopropyl]-carbamate (Intermediate 115, 1.08 g, 3.40 mmols) in 20 mL MeOH and 20 mL THF was added 20 mL of 3M aqueous HCl. The solution was warmed to 35° C. for 3 hours and then stirred for 17 h at 25° C. The reaction was quenched by adjusting the pH of the solution to 12 with 3M aqueous NaOH. The mixture was extracted with Et2O and the combined organic layers were washed with H2O and saturated aqueous NaCl before being dried (MgSO4) and concentrated under reduced pressure. The title compound 613 mg (85%) was used without further purification.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US06713647B2uspto-grants-2004_03