تفاعل #1893

ord-b12632ff90da4c7fbf9aead0149dd2e8

معادلة التفاعل

COc1ccccc1C(=O)c1cc(Cl)ccc1N
2-amino-5-chloro-2'-methoxybenzophenone
O=C([O-])O.[Na+]
sodium bicarbonate
Nc1ccc(Cl)cc1C(=O)c1ccccc1O
2-amino-5-chloro-2'-hydroxybenzophenone
المردود 93.4%

الكواشف

لا شيء

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    درجة الحرارةwas heated for 1 hour
  2. 2
    درجة الحرارةunder reflux
  3. 3
    استخلاصsubjected to extraction with 100 ml of ethyl acetate
  4. 4
    غسيلThe extract solution was washed with water
  5. 5
    تجفيفdried over anhydrous magnesium sulfate
  6. 6
    workup.DISTILLATIONthe solvent was then distilled off under reduced pressure
  7. 7
    أخرىThe residue was purified by means of silica gel column chromatography (eluent, hexane:ethyl acetate=10:1)

الإجراء التجريبي

A mixture of 2.15 g of 2-amino-5-chloro-2'-methoxybenzophenone and 20 ml of 47% hydrogen bromide was heated for 1 hour under reflux. The solution was rendered neutral with sodium bicarbonate, and subjected to extraction with 100 ml of ethyl acetate. The extract solution was washed with water and dried over anhydrous magnesium sulfate; the solvent was then distilled off under reduced pressure. The residue was purified by means of silica gel column chromatography (eluent, hexane:ethyl acetate=10:1) to yield 1.9 g of 2-amino-5-chloro-2'-hydroxybenzophenone as needles, m.p. 51° to 52° C.

المصدر

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