تفاعل #1893
ord-b12632ff90da4c7fbf9aead0149dd2e8
معادلة التفاعل
2-amino-5-chloro-2'-methoxybenzophenone
sodium bicarbonate
→
2-amino-5-chloro-2'-hydroxybenzophenone
المردود 93.4%
الكواشف
لا شيء
المذيبات
ظروف التفاعل
الظروف التفصيلية
See reaction.notes.procedure_details.
المعالجة
- 1درجة الحرارةwas heated for 1 hour
- 2درجة الحرارةunder reflux
- 3استخلاصsubjected to extraction with 100 ml of ethyl acetate
- 4غسيلThe extract solution was washed with water
- 5تجفيفdried over anhydrous magnesium sulfate
- 6workup.DISTILLATIONthe solvent was then distilled off under reduced pressure
- 7أخرىThe 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.