関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Sodium Bicarbonate | HCID 516892 | — |
| 反応物 | Ethyl 4-bromo-2-nitro-6-(trifluoromethyl)phenyl(2,4-dimethoxybenzyl)carbamate | HCID 22327366 | — |
| 触媒 | titanium(III) trichloride | HCID 10313229 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | Ethyl 2-amino-4-bromo-6-(trifluoromethyl)phenyl(2,4-dimethoxybenzyl)carbamate | HCID 22327363 | 100.1% |
反応手順
To a solution of ethyl 4-bromo-2-nitro-6-(trifluoromethyl)phenyl(2,4-dimethoxybenzyl)carbamate (1.204 g) in methanol (90 ml) was added titanium(III) chloride solution (20% wt) (31.5595 g) in an ice bath. The reaction mixture was stirred for 20 minutes at 0° C. To the reaction mixture were added saturated aqueous sodium bicarbonate solution and water, and the mixture was extracted 5 times with ethyl acetate. The organic layer was dried over anhydrous magnesium sulfate, and concentrated in vacuo to give the title compound (1.1345 g, quantitative yield).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06939887B2 |
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| 出典データセット | uspto-grants-2005_09 |
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| ORD ID | ord-f200675a2266465fa60dab2413d8f347 |
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| 出典メモ | uspto-grants-2005_09 |
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