تفاعل #2180

ord-98ad3a1cf50b4a51a88db33c7e3d6103

الكواشف

لا شيء

المذيبات

ظروف التفاعل

درجة الحرارة
0°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    workup.WAITThe resulting mixture was kept at 0° C. for one half hour
  2. 2
    استخلاصThe aqueous suspension was extracted with ether (3×100 ml)
  3. 3
    غسيلthe combined ether layers washed with brine
  4. 4
    أخرىdried
  5. 5
    أخرىyielding the crude product

الإجراء التجريبي

To a suspension of NaH (60% in mineral oil, 340 mg) in dry DMF (75 ml) at 0° C. was added the preceding pyridinone (1.0 g) and the mixture was stirred at 0° C. for one half hour. To the resulting suspension was added 1-bromo-2-pentyne (750 mg) dropwise. The resulting mixture was kept at 0° C. for one half hour and poured into saturated aqueous ammonium chloride (200 ml). The aqueous suspension was extracted with ether (3×100 ml), the combined ether layers washed with brine and dried, yielding the crude product. Trituration with hexane yielded the product as a yellow solid.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US05728694uspto-grants-1998_03