참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Chloride | HCID 312 | — |
| 반응물 | Sodium Iodide | HCID 5238 | — |
| 반응물 | Ethyl Acrylate | HCID 8821 | — |
| 반응물 | 2,4-Dichlorobenzotrifluoride | HCID 9443 | — |
| 반응물 | Triphenylphosphine | HCID 11776 | — |
| 촉매 | Nickel(II) bromide | HCID 278492 | — |
| 용매 | Dimethylformamide | HCID 6228 | — |
| 용매 | Triethylamine | HCID 8471 | — |
| 생성물 | Ethyl 3-chloro-4-trifluoromethylcinnamate | HCID 53835929 | 24.7% |
반응 단계
A suspension of 3.5 g of 2,4-dichlorobenzotrifluoride, 1.28 g of triphenylphosphine, 865 mg of paradium(II) chloride, 2.68 g of sodium iodide, 712 mg of nickel(II) bromide, 4.94 g of triethylamine, and 1.79 g of ethyl acrylate in 16 ml of N,N-dimethylformamide was heated at 140° C. for over night in a sealed tube. The reaction mixture was filtrated off, and the filtrate was concentrated under a reduced pressure. The residue was extracted with ethyl acetate, the extract was washed with water, dried, and evaporated under a reduced pressure. The resulting residue was purified by a silica gel column chromatography to give 1.12 g of ethyl 3-chloro-4-trifluoromethylcinnamate.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 특허 번호 | US05294718 |
|---|
| 출처 데이터셋 | uspto-grants-1994_03 |
|---|
| ORD ID | ord-6626cf1b872c47869f0e7a6cb26ae6f8 |
|---|
| 출처 메모 | uspto-grants-1994_03 |
|---|
