Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Water → 4-[4-(Diethylcarbamoyl-phenyl-methyl)-piperazin-1-yl]-N-(3,5-dimethyl-isoxazol-4-ylmethyl)-3-fluoro-benzamide
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Water | HCID 962 | — |
| 반응물 | Oxalyl chloride | HCID 65578 | — |
| 반응물 | 4-Bromo-3-fluorobenzoic acid | HCID 2773341 | — |
| 반응물 | (Dimethyl-1,2-oxazol-4-yl)methanamine | HCID 11018874 | — |
| 반응물 | 4-Bromo-N-(3,5-dimethyl-isoxazol-4-ylmethyl)-3-fluoro-benzamide | HCID 69304057 | — |
| 용매 | 1,2-Dichloroethane | HCID 11 | — |
| 용매 | Dimethylformamide | HCID 6228 | — |
| 생성물 | 4-[4-(Diethylcarbamoyl-phenyl-methyl)-piperazin-1-yl]-N-(3,5-dimethyl-isoxazol-4-ylmethyl)-3-fluoro-benzamide | HCID 16667230 | 69% |
반응 단계
4-Bromo-N-(3,5-dimethyl-isoxazol-4-ylmethyl)-3-fluoro-benzamide. To a mixture of 4-bromo-3-fluoro-benzoic acid (3.0 mmol) and DMF (0.10 mL) in DCE (10 mL) was added (COCl)2 (4.0 mL) dropwise. After 30 min, the mixture was concentrated and dried under vacuum. The residue was dissolved in DCE (20 mL), treated with C-(3,5-dimethyl-isoxazol-4-yl)-methylamine (3.0 mmol) and TEA (8.0 mmol), and stirred at rt for 16 h. The mixture was treated with H2O (10 mL). The resulting precipitate was collected by filtration to give the title compound (650 mg, 69%).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US08183239B2 |
| 출처 데이터셋 | uspto-grants-2012_05 |
| ORD ID | ord-10aa7b6ad7d0451c86b4cf2781b44f7c |
| 출처 메모 | uspto-grants-2012_05 |