関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Ethanol | HCID 702 | — |
| 反応物 | Sodium Carbonate | HCID 10340 | — |
| 反応物 | HCID 17605790 | HCID 17605790 | — |
| 生成物 | Ethyl 2-((3-bromophenyl)amino)acetate | HCID 302657 | — |
反応手順
A mixture of 21.3 g of 3-bromophenylglycine in 160 cm3 of 6.5N hydrochloric ethanol is heated with stirring for 24 hours at a temperature in the region of 80° C. The reaction medium is filtered and the filter cake is then washed with twice 30 cm3 of ethanol. The filtrate is concentrated under reduced pressure (5 kPa) at a temperature in the region of 40° C. An oil is obtained, which is basified by addition of aqueous sodium carbonate solution. The mixture is extracted with 3 times 100 cm3 of ethyl acetate. The extracts are combined, washed with twice 100 cm3 of aqueous sodium chloride solution, dried over sodium sulfate, filtered and then concentrated under reduced pressure (5 kPa) at a temperature in the region of 40° C. 4.7 g of ethyl 3-bromophenylglycinate are obtained in the form of a yellow oil. (Rf=0.38 in a 90/5 by volume dichloromethane/methanol mixture, on a Merck 60F254R silica plate).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06420566B2 |
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| 出典データセット | uspto-grants-2002_07 |
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| ORD ID | ord-6f6555e946f1412584db1f555879dd64 |
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| 出典メモ | uspto-grants-2002_07 |
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