تفاعل #4495

ord-e63f4e4c221e4ca7857dee83451d2403

الكواشف

لا شيء

ظروف التفاعل

درجة الحرارة
120°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    درجة الحرارةAfter cooling
  2. 2
    استخلاصthe mixture was extracted with ethyl acetate
  3. 3
    غسيلThe extract was washed with water
  4. 4
    تجفيفdried (MgSO4)
  5. 5
    تركيزconcentrated
  6. 6
    أخرىThe residue was purified by chromatography on silica gel with ethyl ether-hexane (1:9)

الإجراء التجريبي

A mixture of benzamide (60.0 g) and ethyl 4-chloroacetoacetate (49.4 g) was heated at 120° C. for 2 hours. After cooling, aqueous sodium bicarbonate solution was added thereto and the mixture was extracted with ethyl acetate. The extract was washed with water, dried (MgSO4) and concentrated. The residue was purified by chromatography on silica gel with ethyl ether-hexane (1:9) to yield ethyl 2-phenyl-4-oxazoleacetate as an oil (26.4 g, 28.0%). NMR (CDCl3)δ: 1.27 (3H, t, J=7 Hz), 3.68 (3H, s), 4.15 (2H, q, J=7 Hz), 7.4 (3H, m), 7.67 (1H, s), 8.0 (2H, m).

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US04725610uspto-grants-1988_02