تفاعل #340244
ord-617be5223ca14dafa4ffe2639fa7320f
معادلة التفاعل
1-aminocyclohexanecarboxylic acid
tetrahydrofuran-methanol
(trimethylsilyl) diazomethane
→
1-amino-1-methoxy-carbonylcyclohexane
المردود 52.0%
الكواشف
لا شيء
ظروف التفاعل
الظروف التفصيلية
See reaction.notes.procedure_details.
المعالجة
- 1درجة الحرارةcooling
- 2تركيزThe reaction mixture was concentrated in vacuo and to the residue
- 3workup.ADDITIONwas added diethyl ether-hexane (1/1)
- 4workup.ADDITIONThereto was added 4M HCl-ethyl acetate (1.05 mL)
- 5ترشيحthe precipitates were collected by filtration
- 6أخرىdried
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.