반응 #1736800

ord-14ce496bf3994918a22328ad63f6768d

시약

없음

반응 조건

온도
-111°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도The solution was then warmed to -80° C.
  2. 2
    workup.STIRRINGstirred for 18 hours at this temperature
  3. 3
    온도slowly warmed to room temperature
  4. 4
    여과The resultant solution was filtered
  5. 5
    기타evaporated to dryness
  6. 6
    기타giving a dark brown solid
  7. 7
    기타The latter gave
  8. 8
    기타a broad metal-hydride absorption band in the infrared region at 1800 cm-1

실험 절차

A solution of potassium naphthalene was prepared from potassium (110 mg) and naphthalene (400 mg), in tetrahydrofuran (40 ml). This was added to a suspension of [(Ph2CH3P)2RuCl]2H (780 mg) in 40 ml of tetrahydrofuran, cooled to -111° C. The reducing metal arene solution was added slowly, and the reaction mixture, at -111° C. was vigorously agitated throughout the addition. The solution was then warmed to -80° C., and stirred for 18 hours at this temperature, then slowly warmed to room temperature. The resultant solution was filtered and evaporated to dryness giving a dark brown solid. The latter gave a broad metal-hydride absorption band in the infrared region at 1800 cm-1. On the basis of the elemental analyses of this crude product, we regard the composition as being [(Ph2CH3P)3RuH]-K+.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US04418227uspto-grants-1983_11