تفاعل #735995

ord-dafb20b22f204cfb81c4ce25c24530f6

المذيبات

ظروف التفاعل

درجة الحرارة
90°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    درجة الحرارةto cool to room temperature
  2. 2
    ترشيحInsoluble materials were filtered
  3. 3
    استخلاصfollowed by extraction with ethyl acetate
  4. 4
    تجفيفThe extract was dried over anhydrous magnesium sulfate
  5. 5
    تركيزconcentrated
  6. 6
    غسيلThe residue was washed with petroleum ether and carbon tetrachloride

الإجراء التجريبي

A suspension of electrolytic iron powder (3.5 g) in a 5% aqueous acetic acid solution was heated to 90° C., and a solution of 4-chloro-2-fluoro-5-(2-propynyloxy)nitrobenzene (5.7 g) in acetic acid (40 ml) was dropwise added thereto at the same temperature. The resultant mixture was stirred at 90°-105° C. for 1 hour and allowed to cool to room temperature. Water (200 ml) was added thereto. Insoluble materials were filtered, and the filtrate was neutralized, followed by extraction with ethyl acetate. The extract was dried over anhydrous magnesium sulfate and concentrated. The residue was washed with petroleum ether and carbon tetrachloride to obtain 3.6 g of 4-chloro-2-fluoro-5-(2-propynyloxy)aniline. M.P. 61.0°-61.5° C.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US04736068uspto-grants-1988_04