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Pyridine → Methyl 3-chloro-4-{[(4-nitrophenoxy)carbonyl]amino}benzoate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Pyridine | HCID 1049 | — |
| 反応物 | Dichloromethane | HCID 6344 | — |
| 反応物 | 4-Nitrophenyl chloroformate | HCID 82129 | — |
| 反応物 | Methyl 4-Amino-3-chlorobenzoate | HCID 1515284 | — |
| 溶媒 | Chloroform | HCID 6212 | — |
| 生成物 | Methyl 3-chloro-4-{[(4-nitrophenoxy)carbonyl]amino}benzoate | HCID 59178754 | — |
反応手順
A 3.5 g portion of 4-nitrophenyl chlorocarbonate was added at 0° C. to a 30 ml dichloromethane suspension of 3 g of methyl 4-amino-3-chlorobenzoate and 4 ml of pyridine and stirred at room temperature for 2Hours. The reaction solution was diluted with chloroform and washed with 1 M hydrochloric acid, water, saturated sodium bicarbonate aqueous solution, water and saturated brine in that order, and the organic layer was dried with anhydrous sodium sulfate. This was concentrated under a reduced pressure, and the thus obtained residue was recrystallized from hexane-ethyl acetate to obtain 4.23 g of methyl 3-chloro-4-{[(4-nitrophenoxy)carbonyl]amino}benzoate as a pale brown powder.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07585886B2 |
| 出典データセット | uspto-grants-2009_09 |
| ORD ID | ord-5af8aeb32cf54573a24ddac1c50705c3 |
| 出典メモ | uspto-grants-2009_09 |