تفاعل #56535

ord-ff0f3baf7efb4b36a3c39f27a020076f

الكواشف

لا شيء

المذيبات

ظروف التفاعل

درجة الحرارة
30°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    غسيلSodium hydride (0.13 moles as a 50% dispersion in mineral oil) is washed with 100 ml
  2. 2
    أخرىof dry n-hexane to remove the mineral oil
  3. 3
    workup.ADDITIONTo this sodium hydride suspension is added dropwise at room temperature
  4. 4
    workup.ADDITIONWhen the addition
  5. 5
    أخرىthe resultant reaction mixture
  6. 6
    استخلاصextracted with (3×200 ml.) of ether
  7. 7
    غسيلThe combined ether extracts are washed, with water, dilute hydrochloric acid, saturated sodium, bicarbonate solution saturated sodium chloride solution
  8. 8
    تجفيفdried over magnesium sulfate
  9. 9
    أخرىThe solvent is evaporated
  10. 10
    أخرىto give 39.8 g

الإجراء التجريبي

Sodium hydride (0.13 moles as a 50% dispersion in mineral oil) is washed with 100 ml. of dry n-hexane to remove the mineral oil, then blanketed with dry nitrogen and suspended in 250 ml. of freshly distilled tetrahydrofuran. To this sodium hydride suspension is added dropwise at room temperature, a solution of 2,4-dichlorobenzyl cyanide (25 g., 0.13 mole) dissolved in 100 ml. of tetrahydrofuran. When the addition is completed the temperature is maintained at 30° C. for an additional 0.5 hours. A solution of n-octylbromide (27 g., 0.14 mole) is then added dropwise and the resultant reaction mixture is stirred at 40° C. overnight under nitrogen. The reaction mixture is poured into 1 liter of water and extracted with (3×200 ml.) of ether. The combined ether extracts are washed, with water, dilute hydrochloric acid, saturated sodium, bicarbonate solution saturated sodium chloride solution, and dried over magnesium sulfate. The solvent is evaporated to give 39.8 g. (100%) of product.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US04225723uspto-grants-1980_09