関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Pyridine | HCID 1049 | — |
| 反応物 | Bromine | HCID 24408 | — |
| 反応物 | Dimethyl aminoterephthalate | HCID 79336 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | Dimethyl 6-amino-4-bromo-terephthalate | HCID 68932527 | — |
反応手順
10.5 g (50 mmol) dimethyl amino-terephthalate and 8.1 ml (100 mmol) pyridine are dissolved in 175 ml dichloromethane and at −16° C. a solution of 2.7 ml (52.5 mmol) bromine in 25 ml dichloromethane is added dropwise. It is stirred for 4 hours at 0° C. and then heated overnight to ambient temperature. The mixture is added to ice water, washed three times with water and then dried over magnesium sulphate and evaporated down. The crude product is recrystallised from ethanol.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07429597B2 |
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| 出典データセット | uspto-grants-2008_09 |
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| ORD ID | ord-a137e12451464b238fb9096e7c5a5528 |
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| 出典メモ | uspto-grants-2008_09 |
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