تفاعل #63342

ord-ebcad93417234d96a6e4d773844c10df

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    أخرىevaporated to a red oil which
  2. 2
    workup.DISSOLUTIONwas dissolved in ethyl acetate
  3. 3
    غسيلwashed with sodium bicarbonate solution
  4. 4
    أخرىevaporated
  5. 5
    أخرىto leave an oil

الإجراء التجريبي

N'-Cyano-N-[3-[3-(1,3-dioxolan-2-yl)phenoxy]propyl]-1-methyl-2-(phenylmethylene)hydrazinecarboximidamide (18.2 g) in tetrahydrofuran (150 ml) was treated with 5N hydrochloric acid (30 ml) at 30° C. for 30 mins. Triethylamine (20 ml) was added followed by sodium borohydride (8.0 g). The resulting mixture was stirred at room temperature for 14 hrs, diluted with ethyl acetate (150 ml) and evaporated to a red oil which was dissolved in ethyl acetate, washed with sodium bicarbonate solution and evaporated to leave an oil. This oil was treated with etheral hydrogen chloride to give the title compound as a white solid (8 g). m.p. 148°-9°. TLC silica, ethyl acetate, water, isopropanol 0.88 ammonia (25:8:15:2) Rf 0.56.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US04764612uspto-grants-1988_08