تفاعل #321737

ord-2ab8363c12684a60ab978844d4e97c09

الكواشف

لا شيء

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    درجة الحرارةThe mixture was heated
  2. 2
    درجة الحرارةunder reflux for 48 hours
  3. 3
    أخرىthe cooled reaction mixture
  4. 4
    ترشيحthe white precipitate filtered off
  5. 5
    غسيلThe aqueous filtrate was then washed with diethyl ether (4×70 ml)
  6. 6
    غسيلthe combined extracts were then washed with water (50 ml)
  7. 7
    تجفيفdried (MgSO4)
  8. 8
    ترشيحfiltered
  9. 9
    أخرىevaporated
  10. 10
    أخرىto give a white solid
  11. 11
    أخرىdried thoroughly
  12. 12
    أخرىrecrystallised (glacial acetic acid)
  13. 13
    تجفيفdried 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).

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US05595682uspto-grants-1997_01