反応 #987486

ord-22cc07019ac546f5b934762c10a3adb4

溶媒

反応条件

温度
70°CELSIUS
詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    workup.DISSOLUTIONdissolution
  2. 2
    温度the reaction is cooled down to room temperature
  3. 3
    濃縮concentrated in vacuo
  4. 4
    その他the crude product is purified by chromatography on silicagel (CH2Cl2/MeOH: 95/05 (v/v))

実験手順

In a three necked flask, under argon, a suspension of 2-[4-amino-2-oxo-1-pyrrolidinyl]butanamide 393 (6.99 g, 0.037 mol.), dimethoxytetrahydrofurane (5.53 g, 0.041 mol.), pyridine (50.6 ml) and AcOH (36 ml) is warmed to 70° C. and dissolution occurs. After 2 h at this temperature, the reaction is cooled down to room temperature, concentrated in vacuo and the crude product is purified by chromatography on silicagel (CH2Cl2/MeOH: 95/05 (v/v)) to afford 223 as an oil (2.67 g, 30.1%). 5.7. Bromination of 4-pyrrolyl-pyrrolidin-2-one 223

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US07358276B2uspto-grants-2008_04