반응 #41166

ord-340ad6098b5640589aae7bb301b76e43

반응 조건

온도
70°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도Upon cooling to room temperature a white solid
  2. 2
    기타precipitated out of solution
  3. 3
    여과The solid was collected by filtration
  4. 4
    세척washed with hexanes
  5. 5
    기타dried

실험 절차

tert-Butyldimethylsilyloxy-cyclohexanone (3.146 g, 97%, 13.36 mmol, CAS #55145-45-4, purchased from Aldrich) was dissolved in hexanes (24 mL). tert-Butyl carbazate (1.80 g, 98%, 13.35 mmol) was added and the mixture was heated at 70° C. for 3 hours. Upon cooling to room temperature a white solid precipitated out of solution. The solid was collected by filtration, washed with hexanes and dried to give N′-[4-(tert-butyl-dimethyl-silanyloxy)-cyclohexylidene]-hydrazinecarboxylic acid tert-butyl ester (4.12 g, 90%).

출처

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