تفاعل #321737
ord-2ab8363c12684a60ab978844d4e97c09
معادلة التفاعل
الكواشف
لا شيء
ظروف التفاعل
الظروف التفصيلية
See reaction.notes.procedure_details.
المعالجة
- 1درجة الحرارةThe mixture was heated
- 2درجة الحرارةunder reflux for 48 hours
- 3أخرىthe cooled reaction mixture
- 4ترشيحthe white precipitate filtered off
- 5غسيلThe aqueous filtrate was then washed with diethyl ether (4×70 ml)
- 6غسيلthe combined extracts were then washed with water (50 ml)
- 7تجفيفdried (MgSO4)
- 8ترشيحfiltered
- 9أخرىevaporated
- 10أخرىto give a white solid
- 11أخرىdried thoroughly
- 12أخرىrecrystallised (glacial acetic acid)
- 13تجفيفdried in vacuo (P2O5, 0.30 mm Hg, 50° C., 5 hours)
الإجراء التجريبي
A mixture of concentrated sulphuric acid (115 ml) and water (115 ml) was added dropwise to a stirred suspension of 4-cyano-4'-hydroxybiphenyl 39 (25.62 g, 131.4 mmol) in glacial acetic acid (400 ml). The mixture was heated under reflux for 48 hours, the cooled reaction mixture was then poured into water (600 ml) with stirring and the white precipitate filtered off. The aqueous filtrate was then washed with diethyl ether (4×70 ml); the combined extracts were then washed with water (50 ml), dried (MgSO4) filtered and evaporated to give a white solid, both crops of product were combined, dried thoroughly and recrystallised (glacial acetic acid) and dried in vacuo (P2O5, 0.30 mm Hg, 50° C., 5 hours).