TERT-BUTYL 4-(N-HYDROXYCARBAMIMIDOYL)-BENZYLCARBAMATE synthesis
- Product Name:TERT-BUTYL 4-(N-HYDROXYCARBAMIMIDOYL)-BENZYLCARBAMATE
- CAS Number:220648-78-2
- Molecular formula:C13H19N3O3
- Molecular Weight:265.31
66389-80-8
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Yield:220648-78-2 99%
Reaction Conditions:
with hydroxylamine hydrochloride;triethylamine in tetrahydrofuran at 75; for 15 h;
Steps:
19.2
(2) To a solution of hydroxylamine hydrochloride (2.24 g, 32.3 mmol) in dimethyl sulfoxide (10.6 mL), triethylamine (4.51 mL, 32.4 mmol) was added and the resulting mixture was stirred at room temperature for an hour. The precipitating salt was filtered and washed with THF. The THF was distilled off under reduced pressure and after adding the foregoing compound (n-2) (1.50 g, 6.46 mmol), the resulting mixture was stirred at 75° C. for 15 hours. The reaction mixture was cooled to room temperature and after adding water, extraction was conducted with ethyl acetate. The organic layer was successively washed with water and saturated brine and dried over anhydrous sodium sulfate. The solvents were distilled off under reduced pressure to give tert-butyl 4-(N′-hydroxycarbamimidoyl)benzylcarbamate (n-3) (amount, 1.70 g; yield, 99%).
References:
US2016/130232,2016,A1 Location in patent:Paragraph 0297
24424-99-5
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10406-25-4
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15996-76-6
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220648-78-2
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