تفاعل #725888

ord-f28df230f2a842f6bd81173f55feb8ca

معادلة التفاعل

CCOC(=O)COc1ccc(NC(C)=O)cc1
(4-Acetylamino-phenoxy)-acetic acid ethyl ester
Cl
hydrochloric acid
Cl.Nc1ccc(OCC(=O)O)cc1
14
المردود 77.6%
Cl.Nc1ccc(OCC(=O)O)cc1
(4-Amino-phenoxy) acetic acid HCl
المردود 77.6%

الكواشف

لا شيء

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 13 (375 g, 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 14 (250 g, 77.6%) as a wheat colored powder. The melting point was found to be 224-226° C. The structure was confirmed with NMR.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US07691364B2uspto-grants-2010_04