참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Hydrochloric Acid | HCID 313 | — |
| 반응물 | 3-Ethylaniline | HCID 11475 | — |
| 반응물 | Diisopropylethylamine | HCID 81531 | — |
| 반응물 | Ethyl bromophenylacetate | HCID 97780 | — |
| 반응물 | Lithium hydroxide, monohydrate | HCID 168937 | — |
| 용매 | Water | HCID 962 | — |
| 용매 | Acetonitrile | HCID 6342 | — |
| 용매 | 1,4-Dioxane | HCID 31275 | — |
| 생성물 | (3-Ethyl-phenylamino)-phenyl-acetic acid hydrochloride | HCID 67425860 | 86% |
반응 단계
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).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 특허 번호 | US08835682B2 |
|---|
| 출처 데이터셋 | uspto-grants-2014_09 |
|---|
| ORD ID | ord-22f063fc9f8c4f459d3047c86dc9734e |
|---|
| 출처 메모 | uspto-grants-2014_09 |
|---|
