化工社化工社 化学情報印刷レポート · 研究参考用
1-Amino-2-propanol → Ethyl 2-(2-hydroxypropylamino)-2-oxo-acetate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 1-Amino-2-propanol | HCID 4 | — |
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | Ethoxalyl chloride | HCID 20884 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | Ethyl 2-(2-hydroxypropylamino)-2-oxo-acetate | HCID 85994322 | 31% |
反応手順
To a stirred solution of 1-amino-propan-2-ol (15.0 g, 199.7 mmol) in DCM (150.0 mL), is added triethylamine (43.30 mL, 299.56 mmol) at 0° C. Chloro-oxo-acetic acid ethyl ester (22.35 mL, 199.7 mmol) is added dropwise to the reaction mixture at 0° C. and the reaction mixture is stirred for 16 hours at room temperature. The mixture is diluted with water (100 mL) at 0° C., extracted with DCM (2×100 mL), washed with water (2×50 mL) and brine (50 mL), dried over Na2SO4, and evaporated to dryness. The crude product is purified by silica gel chromatography, eluting with hexane:ethyl acetate (3.0:7.0) to give the title compound as a pale yellow gel (10.7 g, 31.0%). ESI/MS m/z 176.2 (M+H)+.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08822486B2 |
| 出典データセット | uspto-grants-2014_09 |
| ORD ID | ord-450d4c0fee3549558dbf0a9a1323f99c |
| 出典メモ | uspto-grants-2014_09 |