تفاعل #1895

ord-c2eabdf1be4f4a81a4b9a839ae6cea53

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    استخلاصThe mixture was subjected to extraction with 150 ml of water and 200 ml of ethyl acetate
  2. 2
    غسيلthe ethyl acetate layer was washed with water
  3. 3
    تجفيفdried over anhydrous magnesium sulfate
  4. 4
    workup.DISTILLATIONdistilled off under reduced pressure
  5. 5
    أخرىThe residue was purified by means of silica gel column chromatography (eluent, hexane:ethyl acetate=10:1 to 5:1)

الإجراء التجريبي

In 30 ml of N,N-dimethylformamide was dissolved 5.0 g of 2-amino-5-chloro-2'-hydroxybenzophenone, as obtained in Example 123 (1), to which were added 4.2 g of potassium carbonate and 2.9 ml of benzyl bromide; the mixture was then stirred for 2 hours at room temperature. The mixture was subjected to extraction with 150 ml of water and 200 ml of ethyl acetate, and the ethyl acetate layer was washed with water, dried over anhydrous magnesium sulfate, and distilled off under reduced pressure. The residue was purified by means of silica gel column chromatography (eluent, hexane:ethyl acetate=10:1 to 5:1) to yield 6.4 g of 2-amino-2'-benzyloxy-5-chlorobenzophenone as prism crystals, m.p. 110° to 111° C.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US05726306uspto-grants-1998_03