Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Dimethylformamide → HCID 178509930, 화합물
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Dimethylformamide | HCID 6228 | — |
| 반응물 | 4-(3-bromo-5-chlorophenoxy)-5-chloro-1H-1,2,3-benzotriazole | HCID 178477835 | — |
| 촉매 | Zinc cyanide (Zn(CN)2) | HCID 11186 | — |
| 용매 | Ethyl Acetate | HCID 8857 | — |
| 생성물 | HCID 178509930 | HCID 178509930 | — |
반응 단계
4-(3-bromo-5-chlorophenoxy)-5-chloro-1H-1,2,3-benzotriazole (5.0 g, 14 mmol), tetrakis triphenylphosphine palladium (0) (4.83 g, 4.83 mmol) and zinc cyanide (1.96 g, 16.7 mmol) were suspended in dry DMF (50 mL) under N2 and placed in an oil bath at 90° C. After 2.5 hours, the reaction was allowed to cool to room temperature. The mixture was diluted with EtOAc (300 mL) and washed with water (4×100 mL), dried (MgSO4), filtered and concentrated with silica gel (20 g). This was purified by automated column chromatography on silica gel (120 g), eluting with 0-30% EtOAc/hexanes to deliver the title compound. LRMS (M+1)=304.8.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US07781454B2 |
| 출처 데이터셋 | uspto-grants-2010_08 |
| ORD ID | ord-ca405af8e237421d88ecbd04e65b6f9d |
| 출처 메모 | uspto-grants-2010_08 |