참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Hydrochloric Acid | HCID 313 | — |
| 반응물 | Ethyl 3-(4-bromophenyl)-2-cyanoprop-2-enoate | HCID 367501 | — |
| 반응물 | HCID 178478191 | HCID 178478191 | — |
| 용매 | Toluene | HCID 1140 | — |
| 생성물 | 3-(4-Bromo-phenyl)-3-(4-chloro-phenyl)-2-cyano-propionic acid ethyl ester | HCID 57691397 | 91% |
반응 단계
A solution of 3-(4-bromo-phenyl)-2-cyano-acrylic acid ethyl ester (1.5 g, 5.36 mmol) in dry toluene (12 ml) was added dropwise to 4-chlorophenylmagnesium bromide (0.5 M solution in tetrahydrofuran, 6.96 ml, 6.96 mmol) at 0° C. The reaction mixture was heated to 85° C. for 3 hours, poured onto ice, acidified with 1N HCl and extracted with ethyl acetate. The organic layer was separated, dried (MgSO4), filtered and concentrated, the crude product was purified over flash silica chromatography eluting with petroleum ether to ethyl acetate/petroleum ether (5:95) to afford the desired product (1.91 g, 91% yield). LC/MS: (PS-A2) Rt 3.78 [M+H]+ 391.93.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 특허 번호 | US08541461B2 |
|---|
| 출처 데이터셋 | uspto-grants-2013_09 |
|---|
| ORD ID | ord-c35a67d7d4624111bda5dd2070df42b2 |
|---|
| 출처 메모 | uspto-grants-2013_09 |
|---|