반응 #432762

ord-5ecac440754e443a8b50adbf7fdb0b38

용매

반응 조건

온도
50°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    workup.STIRRINGstirring
  2. 2
    온도The reaction mixture was cooled
  3. 3
    여과filtered
  4. 4
    여과The precipitated product was filtered off
  5. 5
    세척washed thoroughly with water
  6. 6
    기타dried overnight at 80° C.

실험 절차

A suspension of 10.69 parts of ethyl 4-amino-5-cyano-2-methoxybenzoate in 12 parts of a sodium hydroxide solution 50% and 500 parts of water was stirred and heated to 50° C. and stirring was continued for 1 hour at 50°-55° C. The reaction mixture was cooled and filtered. The filtrate was acidified with concentrated hydrochloric acid of pH 1-2. The precipitated product was filtered off, washed thoroughly with water and dried overnight at 80° C., yielding 8.6 parts (93.2%) of 4-amino-5-cyano-2-methoxybenzoic acid; mp. 236.7° C. (intermediate 111).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US05057525uspto-grants-1991_10