反応 #41163
ord-a55d876453f4475cb4c8243c9b31c485
反応方程式
溶媒
反応条件
温度
67.5°CELSIUS
詳細条件
See reaction.notes.procedure_details.
後処理
- 1温度The mixture was cooled
- 2濃縮concentrated in vacuo
- 3温度chilled
- 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.