참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Benzyl Alcohol | HCID 244 | — |
| 반응물 | Pentafluorobenzoic acid | HCID 11770 | — |
| 반응물 | 1,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochloride | HCID 2723939 | — |
| 촉매 | 4-(Dimethylamino)pyridine | HCID 14284 | — |
| 용매 | Dichloromethane | HCID 6344 | — |
| 용매 | Sodium chloride; water | HCID 57417360 | — |
| 생성물 | Pentafluorobenzoic acid, benzyl ester | HCID 517856 | 77.3% |
반응 단계
A solution of 2,3,4,5,6-pentafluorobenzoic acid (15.25 g, 71.9 mmol), 4-dimethylaminopyridine (4.4 g, 36.0 mmol) and benzyl alcohol (7.4 mL, 71.5 mmol) in dichloromethane (150 mL) is cooled to 0° C. under an inert atmosphere. 1-[3-(Dimethylamino)propyl]-3-ethyl carbodiimide hydrochloride (16.7 g, 87.1 mmol) is added and the mixture stirred at 0° C. for 2 hours. The mixture is warmed to ambient temperature, stirred for 24 hours, and then poured into brine. The mixture is extracted with chloroform and the organic phase washed with NaHCO3, dried over Na2SO4, filtered and concentrated under vacuum to yield the title compound as a white solid (16.7 g). This material is used without further purification. 1H NMR (CDCl3): δ 7.49–7.27 (m, 5H), 5.40 (s, 2H).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 특허 번호 | US07094780B1 |
|---|
| 출처 데이터셋 | uspto-grants-2006_08 |
|---|
| ORD ID | ord-0840a894e93d4828b9a71ddc2cef0484 |
|---|
| 출처 메모 | uspto-grants-2006_08 |
|---|
