반응 #41163

ord-a55d876453f4475cb4c8243c9b31c485

시약

없음

반응 조건

온도
67.5°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도The mixture was cooled
  2. 2
    농축concentrated in vacuo
  3. 3
    온도chilled
  4. 4
    여과The crystalline material was collected by filtration

실험 절차

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.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US07728029B2uspto-grants-2010_06