反応 #41163

ord-a55d876453f4475cb4c8243c9b31c485

試薬

なし

反応条件

温度
67.5°CELSIUS
詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    温度The mixture was cooled
  2. 2
    濃縮concentrated in vacuo
  3. 3
    温度chilled
  4. 4
    ろ過The crystalline material was collected by filtration

実験手順

Cyclopentanone (5.000 g, 59.44 mmol; CAS #120-92-3, purchased from Aldrich) was dissolved in hexanes (90 mL). t-Butyl carbazate (7.860 g, 59.47 mmol) was added and the mixture was heated at 65-70° C. for 1 hour. The mixture was cooled and concentrated in vacuo. The residue was taken up in isopropanol (25 mL)-ether (25 mL)-hexanes (50 mL) and chilled. The crystalline material was collected by filtration to give N′-cyclopentyl-hydrazinecarboxylic acid tert-butyl ester (5.51 g; 47%). A second crop (2.62 g, 22%) was collected from the mother liquor.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US07728029B2uspto-grants-2010_06