Carbamic acid, (3-cyanophenyl)-, 1,1-dimethylethyl ester (9CI) synthesis
- Product Name:Carbamic acid, (3-cyanophenyl)-, 1,1-dimethylethyl ester (9CI)
- CAS Number:145878-50-8
- Molecular formula:C12H14N2O2
- Molecular Weight:218.25
24424-99-5
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2237-30-1
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145878-50-8
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Yield:145878-50-8 93.2%
Reaction Conditions:
with triethylamine in tetrahydrofuran; for 48 h;Heating / reflux;
Steps:
15.47
To a solution of 3-amino-benzonitrile (4.7g, 40.0 mmol) in 20OmL THF, was added triethylamine (5.6mL, 40.0 mmol), followed by di-tert-butyl dicarbonate (8.7g, 40.0 mmol). After two days of heating at reflux, the solution was cooled, then partitioned between water and and ethyl acetate. The product was extracted three times with ethyl acetate, washed with aqueous IM HCl and brine, dried over magnesium sulfate, filtered, and concentrated to dryness. The product was purified using silica gel chromatography (elution with 10% hexane/90% ethyl acetate) to provide A (8.3 Ig, 93.2%).
References:
WO2006/44497,2006,A2 Location in patent:Page/Page column 148
24424-99-5
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145878-50-8
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18437-67-7
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145878-50-8
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766-84-7
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917-61-3
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75-65-0
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145878-50-8
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4248-19-5
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6952-59-6
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145878-50-8
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