تفاعل #1672667

ord-d4f1906b43774552872a2795754939db

المذيبات

ظروف التفاعل

درجة الحرارة
100°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    workup.ADDITIONwas added
  2. 2
    استخلاصextracted with ethyl acetate three times
  3. 3
    غسيلThe combined organic phase was washed with water
  4. 4
    تجفيفdried (Na2SO4)
  5. 5
    أخرىevaporated
  6. 6
    أخرىchromatographed on silica gel

الإجراء التجريبي

In 100 ml of dimethylformamide was dissolved 4.4 g (0.0115 mmol) of crude 1-benzyloxycarbonylamidino-4-mesyloxyethyl piperidine and 4.5 g (0.069 mol) of sodium azide was added. The mixture was heated at 100° C. for 2.5 h. It was then poured into water and extracted with ethyl acetate three times. The combined organic phase was washed with water, dried (Na2SO4) and evaporated. The residue was flash chromatographed on silica gel using ethyl acetate/heptane 1/1 as eluent. Yield: 3.0 g (79%).

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US05939392uspto-grants-1999_08