化工社化工社 化学情報印刷レポート · 研究参考用
Triethylamine → 2,6-Bis-(2-benzyloxy-acetylamino)-hexanoic acid methyl ester
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | Methyl L-lysinate dihydrochloride | HCID 117778 | — |
| 反応物 | Benzyloxyacetyl chloride | HCID 177085 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | 2,6-Bis-(2-benzyloxy-acetylamino)-hexanoic acid methyl ester | HCID 59682487 | 31.8% |
反応手順
To a mixture of L-lysine methyl ester dihydrochloride (50 grams, 214.4 mmol), triethylamine (131 grams, 1.294 moles) in ethyl acetate (750 mL) at room temperature was added benzyloxy acetyl chloride (120 grams, 650.4 mmol) drop wise. The mixture was further stirred at room temperature for 2 hours. The solids were filtered off. The organic phase was washed with 5% sodium bicarbonate (2×100 mL), water (2×100 mL), dried over sodium sulphate and distilled. The crude 2 was purified by column chromatography on silica gel using Benzene:Ethyl acetate (9:1) to get pure 2 (30 grams, 31.8%) as a white powder.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08754135B2 |
| 出典データセット | uspto-grants-2014_06 |
| ORD ID | ord-5e094245c1254f09b39405a0d1cdd61d |
| 出典メモ | uspto-grants-2014_06 |