Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Potassium Phosphate, Tribasic → 1-Benzothiazol-6-yl-4-methyl-3-(4-methyl-pyridin-3-yl)-imidazolidin-2-one
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Potassium Phosphate, Tribasic | HCID 62657 | — |
| 반응물 | 1-N,2-N-dimethylcyclohexane-1,2-diamine | HCID 551074 | — |
| 반응물 | 3-Iodo-4-methylpyridine | HCID 14423513 | — |
| 반응물 | 1-Benzothiazol-6-yl-4-methyl-imidazolidin-2-one | HCID 59636211 | — |
| 촉매 | Copper iodide | HCID 83717 | — |
| 용매 | Methanol | HCID 887 | — |
| 용매 | Chloroform | HCID 6212 | — |
| 용매 | 1,4-Dioxane | HCID 31275 | — |
| 생성물 | 1-Benzothiazol-6-yl-4-methyl-3-(4-methyl-pyridin-3-yl)-imidazolidin-2-one | HCID 49871961 | 16.66% |
반응 단계
Using the same reaction conditions and work up as described in Example 1, step-3,1-benzothiazol-6-yl-4-methyl-imidazolidin-2-one (I-167b: 150 mg, 0.643 mmol) was refluxed with 3-iodo-4-methyl-pyridine (155 mg, 0.708 mmol), copper iodide (12.21 mg, 0.0643 mmol), N,N′-dimethyl-cyclohexane-1,2-diamine (27.39 mg, 0.192 mmol), potassium phosphate (341.5 mg, 1.607 mmol) and 1,4-dioxane (5 mL) at 120° C. for 12 hours to afford the crude product. The reaction was monitored by TLC (10% MeOH in chloroform). Purification by column chromatography on silica gel (3% methanol in chloroform) followed by preparative HPLC afforded 34 mg of the product (16.66% yield).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | USRE045173E1 |
| 출처 데이터셋 | uspto-grants-2014_09 |
| ORD ID | ord-c7f55d5db3414a5da3720921e0304c55 |
| 출처 메모 | uspto-grants-2014_09 |