تفاعل #54965

ord-c6d54deac7e142829d3b2da97761ea92

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    درجة الحرارةheated
  2. 2
    استخلاصextracted with ether
  3. 3
    غسيلThe combined etheral extracts were washed with water
  4. 4
    تجفيفdried (MgSO4)
  5. 5
    تركيزconcentrated in vacuo
  6. 6
    أخرىaffording

الإجراء التجريبي

Methyl 2-[2,3-dihydro-2-ethyl-3-methyl-4-oxo-4H-1-benzopyran-6-yl]propionate (6 g) was dissolved in ethanol (200 ml) and heated to reflux with dilute aqueous sodium bicarbonate solution (50 ml) for eight hours. The reaction mixture was poured into water, acidified and extracted with ether. The combined etheral extracts were washed with water and dried (MgSO4) and concentrated in vacuo affording a mixture of the desired product and starting material which were separated by chromatography on silica gel using dichloromethane/ether mixtures as eluant. The title compound was recrystallised from petroleum ether (bp 40°-60° C.) as a white solid: 1.4 g, mp 114°-115° C.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US04151179uspto-grants-1979_04