참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Dimethylformamide | HCID 6228 | — |
| 반응물 | Cesium carbonate | HCID 10796 | — |
| 반응물 | Methyl 3-chloropropionate | HCID 22321 | — |
| 반응물 | 4-Iodopyrazole | HCID 77022 | — |
| 용매 | Ethyl Acetate | HCID 8857 | — |
| 생성물 | methyl 3-(4-iodo-1H-pyrazol-1-yl)propanoate | HCID 64435500 | — |
반응 단계
To a mixture of 4-iodopyrazole (1.000 g, 5.155 mmol), Cs2CO3 (2.016 g, 6.186 mmol), and DMF (20 mL, 0.2 mol) was added methyl 3-chloropropanoate (758.1 mg, 6.186 mmol) at 0° C. The reaction was heated to 50° C. for 1 h. The material was transferred to a separatory funnel, diluted with EtOAc, and washed with water several times to remove DMF. The organic layer was dry-loaded onto silica gel, and column chromatography was used for purification, eluting with 3:1 Hexanes/EtOAc, affording the title compound as a clear liquid. MS (ES+): m/z=280.95 (100) [MH+]. HPLC: tR=2.91 min (ZQ3, polar—5 min).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 특허 번호 | US08178668B2 |
|---|
| 출처 데이터셋 | uspto-grants-2012_05 |
|---|
| ORD ID | ord-013d4ab7a0e647519da4711fb98ef0af |
|---|
| 출처 메모 | uspto-grants-2012_05 |
|---|
