반응 #352872

ord-5118d3d706d4462c8c54071daaf25c58

반응 방정식

c1ccc(P(c2ccccc2)c2ccccc2)cc1
triphenylphosphine
Clc1ccc(I)cc1
p-chloroiodobenzene
Clc1ccc([P+](c2ccccc2)(c2ccccc2)c2ccccc2)cc1.[I-]
p-chlorophenyltriphenylphosphonium iodide
수율 96.0%

용매

반응 조건

온도
150°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도the reaction mixture was cooled to room temperature
  2. 2
    기타the precipitate was collected on
  3. 3
    여과a filter by suction
  4. 4
    세척The collected precipitate was washed with xylene
  5. 5
    기타dried under reduced pressure at 130° C. for 3 hours

실험 절차

In 100 mL-volume egg-plant type flask, 3.30 g (11.4 mmol) of triphenylphosphine and 3.00 g (12.6 mmol) of p-chloroiodobenzene were dissolved in 40 mL of xylene. To the solution was added 30.0 mg (0.134 mmol) of palladium acetate, and the resulting mixture was stirred at 150° C. for 9.5 hours. After the reaction was complete, the reaction mixture was cooled to room temperature, and the precipitate was collected on a filter by suction. The collected precipitate was washed with xylene and dried under reduced pressure at 130° C. for 3 hours. There was obtained 5.48 g (yield: 87%) of p-chlorophenyltriphenylphosphonium iodide (m.p.: 219°-222° C., elemental analysis: found: C 57.84%, H 3.74%, calculated: C 57.57%, H 3.82%).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US05648510uspto-grants-1997_07