تفاعل #2492358

ord-b1d27f31da5843468f76c9750cfff825

ظروف التفاعل

درجة الحرارة
10°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    workup.DISTILLATIONExcess concentrated hydrochloric acid was distilled off in vacuum
  2. 2
    ترشيحfiltered hot
  3. 3
    ترشيحfiltered
  4. 4
    أخرىdried

الإجراء التجريبي

A mixture (4-acetylamino-phenoxy)-acetic acid ethyl ester 59 (375 grams, 1.582 mmol), in concentrated hydrochloric acid (9.36 liters) was refluxed for 12 hours. Excess concentrated hydrochloric acid was distilled off in vacuum and filtered hot. The mixture was cooled to 10° C., filtered and dried to give pure 60 (250 grams, 77.6%) as a wheat colored powder. The melting point was found to be 224-226° C. The structure was confirmed with NMR. IHNMR (D2O) δ 4.68(s, 2H, OCH2), 3.65(s,3H,ester), 7.0(d,2H,Ar), 7.30(d,2H,Ar

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US08802892B2uspto-grants-2014_08