反応 #576140

ord-56019e87af7e450a89c2c1a2ddb0a408

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    その他flushed with nitrogen for 15 minutes
  2. 2
    workup.ADDITIONTo this was added 11.4 grams of sodium borohydride
  3. 3
    workup.STIRRINGstirring
  4. 4
    workup.ADDITION3.0 grams of sodium borohydride was added
  5. 5
    workup.STIRRINGstirring
  6. 6
    workup.WAITwas continued for 16 hours at room temperature
  7. 7
    workup.ADDITIONTo the resulting mixture was added 170 mL of acetic acid
  8. 8
    温度the mixture was heated at 60° C. for one hour
  9. 9
    workup.ADDITIONTo this mixture was added 120 mL of concentrated hydrochloric acid
  10. 10
    温度heating
  11. 11
    workup.WAITwas continued at 60° C. for one hour
  12. 12
    温度The resulting mixture was cooled to room temperature
  13. 13
    ろ過the resulting solid was collected by filtration
  14. 14
    その他dried

実験手順

A mixture of 20 grams of 7,14-dihydro-3,10-dinonylpentacene-5,12-dione and 400 mL of 2-methoxyethyl ether was stirred and flushed with nitrogen for 15 minutes. To this was added 11.4 grams of sodium borohydride and stirring was continued at 60° C. for 18 hours. The resulting mixture was cooled to room temperature, 3.0 grams of sodium borohydride was added, and stirring was continued for 16 hours at room temperature. To the resulting mixture was added 170 mL of acetic acid, and the mixture was heated at 60° C. for one hour. To this mixture was added 120 mL of concentrated hydrochloric acid and heating was continued at 60° C. for one hour. The resulting mixture was cooled to room temperature and the resulting solid was collected by filtration and dried to give 2,9-dinonylpentacene.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US06974877B2uspto-grants-2005_12