関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | 3-Ethylaniline | HCID 11475 | — |
| 反応物 | Diisopropylethylamine | HCID 81531 | — |
| 反応物 | Ethyl bromophenylacetate | HCID 97780 | — |
| 反応物 | Lithium hydroxide, monohydrate | HCID 168937 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 溶媒 | 1,4-Dioxane | HCID 31275 | — |
| 生成物 | (3-Ethyl-phenylamino)-phenyl-acetic acid hydrochloride | HCID 67425860 | 86% |
反応手順
Ethyl 2-bromo-2-phenylacetate (0.29 mL, 1.64 mmol), 3-ethylaniline (0.31 mL, 2.47 mmol), and N-ethyl-N-isopropylpropan-2-amine (0.43 mL, 2.47 mmol) are dissolved in acetonitrile (5 mL) and stirred under MW irradiation at 100° C. for 1 hour (Conversion complete by UPLC/MS-UV). Lithium hydroxide hydrate (207 mg, 4.94 mmol) and water (3 mL) are added and the mixture is stirred at RT for 16 hours. 4M HCl in dioxane is added until pH 1 and the solvents are evaporated. The residue is suspended in water, sonicated, cooled at 0° C. and filtered under suction. The recovered white solid is dried under vacuum at 40° C. overnight (414 mg, 86% yield).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US08835682B2 |
|---|
| 出典データセット | uspto-grants-2014_09 |
|---|
| ORD ID | ord-22f063fc9f8c4f459d3047c86dc9734e |
|---|
| 出典メモ | uspto-grants-2014_09 |
|---|
