참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Water | HCID 962 | — |
| 반응물 | 3',4'-Dimethoxycinnamic acid | HCID 16848 | — |
| 반응물 | 1,1'-Carbonyldiimidazole | HCID 68263 | — |
| 반응물 | HCID 178458070 | HCID 178458070 | — |
| 용매 | Dimethylformamide | HCID 6228 | — |
| 생성물 | HCID 67396938 | HCID 67396938 | — |
반응 단계
3-(3,4-Dimethoxy-phenyl)-acrylic acid (compound of Example 2, Method A, Step 1; 4 g, 19.21 mmol) was dissolved in DMF (30 mL) to which 1,1′-Carbonyldiimidazole (CDI) (4.04 g, 24.97 mmol) was added and the reaction mixture was stirred at room temperature. At the end of 3 h, N-hydroxy-propionamidine (2.03 g, 23.05 mmol) was added and the reaction mixture was stirred at room temperature for 8 h. After completion of the reaction, additional CDI (4.04 g, 24.97 mmol) was added and the reaction mixture was refluxed at 110° C. to 120° C. for 8 h to effect cyclodehydration. After evaporation of DMF, the residue obtained was cooled to room temperature followed by addition of water (25 mL) and extracted with ethyl acetate (3×15 mL). The combined organic layers were washed with water (2×10 mL) and brine (10 mL), dried over anhydrous sodium sulfate and concentrated to afford the title compound.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 특허 번호 | US08629277B2 |
|---|
| 출처 데이터셋 | uspto-grants-2014_01 |
|---|
| ORD ID | ord-4e09fbef66814f7896dbb8ea0c3eb129 |
|---|
| 출처 메모 | uspto-grants-2014_01 |
|---|