Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
3-Bromopyridine → 3-Benzothiazol-6-yl-1-pyridin-3-yl-4-trifluoromethyl-imidazolidin-2-one
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | 3-Bromopyridine | HCID 12286 | — |
| 반응물 | Potassium Phosphate, Tribasic | HCID 62657 | — |
| 반응물 | 1-N,2-N-dimethylcyclohexane-1,2-diamine | HCID 551074 | — |
| 반응물 | 1-Benzothiazol-6-yl-5-trifluoromethyl-imidazolidin-2-one | HCID 59636203 | — |
| 촉매 | Copper iodide | HCID 83717 | — |
| 용매 | Ethyl Acetate | HCID 8857 | — |
| 용매 | 1,4-Dioxane | HCID 31275 | — |
| 생성물 | 3-Benzothiazol-6-yl-1-pyridin-3-yl-4-trifluoromethyl-imidazolidin-2-one | HCID 49872558 | 45.2% |
반응 단계
Using the same reaction conditions and work up as described in Example 1, step-3,1-benzothiazol-6-yl-5-trifluoromethyl-imidazolidin-2-one (I-172b: 0.1 g, 0.0004 mol) was refluxed with 3-bromo-pyridine (0.085 g, 0.0005 mol), copper iodide (0.0076 g, 0.00004 mol), N,N′-dimethyl-cyclohexane-1,2-diamine (0.017 g, 0.00012 mol), potassium phosphate (0.22 g, 0.0012 mol) and 1,4-dioxane (20 mL) at 120° C. for 12 hours to afford the crude product. The reaction was monitored by TLC (100% ethyl acetate). Purification by column chromatography on silica gel (2% methanol in DCM) afforded 54 mg of the product (45.2% yield).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | USRE045173E1 |
| 출처 데이터셋 | uspto-grants-2014_09 |
| ORD ID | ord-dc31d96234044d42853fa7bc593206eb |
| 출처 메모 | uspto-grants-2014_09 |