تفاعل #159742

ord-171553ac0f9f49ccadb845cb054be1ea

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    workup.STIRRINGthe reaction mixture was stirred for another 4 h at room temperature
  2. 2
    أخرىThe reaction was quenched by addition of water
  3. 3
    استخلاصextracted with ethyl acetate (50×2 mL)
  4. 4
    غسيلThe organic layer was washed with water (20 mL)
  5. 5
    تركيزconcentrated
  6. 6
    أخرىpurified by silica gel column chromatography

الإجراء التجريبي

To a stirred solution of 3,4-dihydro-2H-benzo[1,4]oxazine (5 g, 37.0 mmol) in DMF (20 mL) was added potassium tert-butoxide (6.22 g, 55.55 mmol) at 0° C. After stirring for 5 min, bromo-cyclopropane (4.44 mL, 55.55 mmol) was added and the reaction mixture was stirred for another 4 h at room temperature. The reaction was quenched by addition of water and extracted with ethyl acetate (50×2 mL). The organic layer was washed with water (20 mL), concentrated and purified by silica gel column chromatography to furnish 4-Cyclopropyl-3,4-dihydro-2H-benzo[1,4]oxazine (4.42 g).

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US08828951B2uspto-grants-2014_09