化工社化工社 化学情報印刷レポート · 研究参考用
ethyl N-(2,3-dichloro-6-nitrobenzyl)glycine hydrochloride → ethyl-N-(6-amino-2,3-dichlorobenzyl)glycine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | ethyl N-(2,3-dichloro-6-nitrobenzyl)glycine hydrochloride | HCID 66640009 | — |
| 触媒 | Platinum | HCID 23939 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | ethyl-N-(6-amino-2,3-dichlorobenzyl)glycine | HCID 67080112 | 72% |
反応手順
A solution of 0.344 g of ethyl N-(2,3-dichloro-6-nitrobenzyl)glycine hydrochloride (compound VI) in 1.5 mL of water and 1.5 mL ethanol (with 5% isopropanol) was stirred and 5% sulfided platinum on carbon under hydrogen (50 to 100 psi) for 16 hours. The catalyst was removed by filtration. The filtrate concentrated, diluted with water and toluene, and basified (aqueous sodium hydroxide or potassium carbonate) to pH 9-10. The organic phase was separated, concentrated, and the crude material purified by low-temperature recrystallization from toluene in hexane to give compound I in 72% yield.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06653500B2 |
| 出典データセット | uspto-grants-2003_11 |
| ORD ID | ord-5ecaf55e573e49b5b990f95c786a5cfc |
| 出典メモ | uspto-grants-2003_11 |