Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Dimethylamine → 2-chloro-4,5-difluoro-N,N-dimethylbenzamide
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Dimethylamine | HCID 674 | — |
| 반응물 | Tetrahydrofuran | HCID 8028 | — |
| 반응물 | Triethylamine | HCID 8471 | — |
| 반응물 | 1-Chloro-N,N-2-trimethylpropenylamine | HCID 640792 | — |
| 반응물 | 2-Chloro-4,5-difluorobenzoic acid | HCID 737171 | — |
| 용매 | Hydrochloric Acid | HCID 313 | — |
| 용매 | Dichloromethane | HCID 6344 | — |
| 생성물 | 2-chloro-4,5-difluoro-N,N-dimethylbenzamide | HCID 59346904 | 96.8% |
반응 단계
A solution of 2-chloro-4,5-difluorobenzoic acid (385 mg, 2.0 mmol) in DCM (5 mL) was treated with (1-chloro-2-methylprop-1-en-1-yl)dimethylamine (293 mg, 2.2 mmol) and stirred under argon for 1 hour. The mixture was then treated with triethylamine (0.56 mL, 4.0 mmol) and a 2M solution of dimethylamine in THF (1.2 mL, 2.4 mmol), and stirred for 18 hours. The mixture was diluted with DCM (5 mL) and 2M hydrochloric acid (4 mL) and separated. The organic layer was dried (MgSO4), filtered and concentrated in vacuo to afford the title compound (425 mg). The residue was used without further purification.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US07745475B2 |
| 출처 데이터셋 | uspto-grants-2010_06 |
| ORD ID | ord-29d4985e8b5643428721490fac721520 |
| 출처 메모 | uspto-grants-2010_06 |