تفاعل #340244

ord-617be5223ca14dafa4ffe2639fa7320f

معادلة التفاعل

NC1(C(=O)O)CCCCC1
1-aminocyclohexanecarboxylic acid
OCC1CCCO1
tetrahydrofuran-methanol
C[Si](C)(C)C=[N+]=[N-]
(trimethylsilyl) diazomethane
COC1(N)CCCCC1=C=O
1-amino-1-methoxy-carbonylcyclohexane
المردود 52.0%

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    درجة الحرارةcooling
  2. 2
    تركيزThe reaction mixture was concentrated in vacuo and to the residue
  3. 3
    workup.ADDITIONwas added diethyl ether-hexane (1/1)
  4. 4
    workup.ADDITIONThereto was added 4M HCl-ethyl acetate (1.05 mL)
  5. 5
    ترشيحthe precipitates were collected by filtration
  6. 6
    أخرىdried

الإجراء التجريبي

A solution of 1-aminocyclohexanecarboxylic acid (600 mg) in tetrahydrofuran-methanol was stirred under ice-cooling. Thereto was added dropwise a (trimethylsilyl) diazomethane solution (4.2 mL) and the mixture was stirred overnight. The reaction mixture was concentrated in vacuo and to the residue was added diethyl ether-hexane (1/1). Thereto was added 4M HCl-ethyl acetate (1.05 mL) and the precipitates were collected by filtration and dried to give 1-amino-1-methoxy-carbonylcyclohexane (423 mg, yield: 52%) as a white powder.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US07872006B2uspto-grants-2011_01