تفاعل #50871

ord-32fdaef34b434ee89b0bff3ed1e90296

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    غسيلit was washed
  2. 2
    استخلاصextracted with ethyl acetate
  3. 3
    تجفيفdried over sodium sulfate
  4. 4
    ترشيحfiltered
  5. 5
    أخرىevaporated to dryness
  6. 6
    أخرىPurification by chromatography

الإجراء التجريبي

To 500 mg of diacid (Example 20, Step 4) in dichloromethane (39 mL) and acetonitrile (9.9 mL) at 0° C. was added 2-chloro-1-methylpyridinium iodide (315 mg). After 15 min triethylamine (170 μL) and 10 mL of a saturated solution of ammonia in ether were added. The solution was stirred 1 hr at room temperature then it was washed with acidified 25% ammonium acetate, extracted with ethyl acetate, dried over sodium sulfate, filtered and evaporated to dryness. Purification by chromatography afforded the title compound.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US05428171uspto-grants-1995_06