반응 #560723

ord-084d1dfa68ce48999479024d7312253c

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    workup.ADDITIONhere were added trisacetylacetonatocobalt (catalyst weight: 3.0 g)
  2. 2
    기타After the reaction system was purged with hydrogen twice
  3. 3
    온도it was heated
  4. 4
    기타kept at 80° C. under a hydrogen
  5. 5
    기타When four hours
  6. 6
    기타to terminate
  7. 7
    기타the reaction

실험 절차

An autoclave with an inner volume of 5 L was charged with 3 L of the decene oligomer produced in (a) in nitrogen gas stream, and here were added trisacetylacetonatocobalt (catalyst weight: 3.0 g) dissolved in toluene and triisobutylaluminum (30 mmol) diluted with toluene. After the reaction system was purged with hydrogen twice, it was heated and kept at 80° C. under a hydrogen pressure of 0.9 MPa. Hydrogenation immediately proceeded exothermically. When four hours passed after the reaction started, the temperature was lowered to terminate the reaction. The pressure was released, the reaction mixture was taken out of the autoclave, and the fraction of boiling at 240 to 270° C. under 530 Pa (desired compound) was isolated by simple distillation.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US08637438B2uspto-grants-2014_01