반응 #93855

ord-901d954f193c43aca74ff7cd531634b3

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타is submitted to hydrogenation at atmospheric pressure and room temperature
  2. 2
    기타After the absorption of 1200 ml of hydrogen the catalysts
  3. 3
    기타are removed by filtration
  4. 4
    농축The solution is concentrated by evaporation in vacuo of most of the solvent
  5. 5
    기타whereafter the product crystallizes as white crystals melting at 152°-154° C

실험 절차

A mixture of 205 g of 2,2-dimethyl-1-ethinyl-7-methoxy-3-(N-methyl-p-toluenesulphonamido)-1,2,3,4-tetrahydro-1-naphthol, 0.8 g of 0,5% palladium on calcium carbonate, 0.8 g 5% palladium on charcoal and 1000 ml of ethyl acetate is submitted to hydrogenation at atmospheric pressure and room temperature. After the absorption of 1200 ml of hydrogen the catalysts are removed by filtration. The solution is concentrated by evaporation in vacuo of most of the solvent, whereafter the product crystallizes as white crystals melting at 152°-154° C. Yield 95%.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US04128548uspto-grants-1978_12