تفاعل #1747341

ord-2fb5f3923dbe497787edbd608a630467

الكواشف

لا شيء

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    درجة الحرارةto reflux temperature under nitrogen for 3 hours
  2. 2
    أخرىthe solvent was removed under vacuum
  3. 3
    أخرىto give a thick brown oil, which
  4. 4
    أخرىwas triturated with five 35 ml portions of refluxing ethyl acetate
  5. 5
    درجة الحرارةcooled to room temperature
  6. 6
    ترشيحThe precipitated solids were filtered
  7. 7
    غسيلwashed with ethyl acetate and vacuum
  8. 8
    تجفيفdried over phosphorous pentoxide

الإجراء التجريبي

N-furfurylthiourea (0.82 grams, 0.005 moles) and α-bromopropiophenone (1.07 grams, 0.005 moles, Aldrich Chem. Co.) in 11 ml absolute ethanol were heated to reflux temperature under nitrogen for 3 hours. After cooling to room temperature, the solvent was removed under vacuum to give a thick brown oil, which was triturated with five 35 ml portions of refluxing ethyl acetate. The ethyl acetate was reduced in volume to about 25 ml and cooled to room temperature. The precipitated solids were filtered, washed with ethyl acetate and vacuum dried over phosphorous pentoxide, yielding 0.585 grams (33%) of 2-furfurylamino-5-methyl-4-phenyl-thiazole hydrobromide, m.p. 150°-153° C.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US04307106uspto-grants-1981_12