تفاعل #4347

ord-b37197377f3049a1b8bb4c506a8c3f2c

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    workup.ADDITIONAfter completion of the dropwise addition
  2. 2
    ترشيحThe crystals thus deposited were collected by filtration

الإجراء التجريبي

8.6 g of the azo obtained in step (2) above, 35 ml of acetonitrile, and 8.6 ml of N,N-dimethylacetamide were put into a 100 ml three-necked flask and 8.6 ml of phosphorus oxychloride was added dropwise to the mixture at a temperature of 50° C. or below. After completion of the dropwise addition, the mixture was stirred for 30 minutes and then poured into ice water. The crystals thus deposited were collected by filtration.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US04725531uspto-grants-1988_02