تفاعل #55745

ord-72bd60edce5b4c00965ff9f142800b3b

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    workup.ADDITIONwere added dropwise
  2. 2
    درجة الحرارةunder reflux
  3. 3
    درجة الحرارةafter cooling
  4. 4
    غسيلit was washed with water, dilute hydrochloric acid
  5. 5
    تجفيفa sodium bicarbonate solution and dried over sodium sulfate

الإجراء التجريبي

10.4 g of 2-ethoxy-4-amino-benzoic acid ethyl ester were suspended in a mixture of 6.8 ml of triethylamine and 200 ml of toluene and 10.3 g of 5-chloro-2-methoxy-benzoyl chloride dissolved in a small amount of toluene were added dropwise. The whole was stirred for 3 hours under reflux and, after cooling, it was washed with water, dilute hydrochloric acid and a sodium bicarbonate solution and dried over sodium sulfate. Upon concentration of the solution under reduced pressure, the 2-ethoxy-4-(5-chloro-2-methoxy-benzamido)-benzoic acid ethyl ester was obtained in the form of a solid product having a crude melting point of 108°-111° C.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US04221815uspto-grants-1980_09