تفاعل #1496725

ord-dac9481abc714010ba21cf2f5cbac49c

الكواشف

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المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    درجة الحرارةcooling
  2. 2
    workup.STIRRINGthe mixture was stirred overnight
  3. 3
    تركيزThe reaction mixture was concentrated in vacuo
  4. 4
    workup.ADDITIONto the residue were added successively diethylether-hexane (1/1)
  5. 5
    ترشيحThe precipitates were collected by filtration
  6. 6
    أخرىdried

الإجراء التجريبي

To a solution of 1-aminocyclohexanecarboxylic acid (600 mg) in tetrahydrofuran-methanol was added dropwise trimethylsilyl diazomethane (4.2 mL) under ice-cooling and stirring, and the mixture was stirred overnight. The reaction mixture was concentrated in vacuo, and to the residue were added successively diethylether-hexane (1/1) and a solution of 4N hydrochloric acid in ethyl acetate (1.05 mL). The precipitates were collected by filtration and dried to give methyl 1-amino-cyclohexanecarboxylate (423 mg, yield: 52%) as a white powder.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US08921380B2uspto-grants-2014_12