تفاعل #74607

ord-e0460eb9b009438f88eda994a318d272

الكواشف

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المذيبات

ظروف التفاعل

درجة الحرارة
0°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    workup.WAITfor 2 hours at room temperature
  2. 2
    ترشيحThe mixture was filtered
  3. 3
    غسيلwashing the solid with acetone (200.0 mL)
  4. 4
    تركيزThe filtrate was carefully concentrated in vacuo (at 400 mbar)
  5. 5
    أخرىThe crude material was purified by flash column chromatography
  6. 6
    غسيلeluting with pentane:diethylether (1:1, by volume)

الإجراء التجريبي

To a mixture of pyrazole (10 g, 0.150 mol) and potassium carbonate (22.3 g, 0.162 mol) in acetone (200.0 mL), cooled to 0° C. under nitrogen, was added chloromethyl ethyl ether (15.0 mL, 0.162 mol) via syringe over a period of 20 minutes. The reaction was stirred for 30 minutes at 0° C. and then for 2 hours at room temperature. The mixture was filtered, washing the solid with acetone (200.0 mL). The filtrate was carefully concentrated in vacuo (at 400 mbar). The crude material was purified by flash column chromatography eluting with pentane:diethylether (1:1, by volume) to afford the title compound as a colourless oil, 9.3 g, 50% yield.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US08541588B2uspto-grants-2013_09