참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Ethylenediamine | HCID 3301 | — |
| 반응물 | 2-Methylpyridine-3-carbonitrile | HCID 4738308 | — |
| 반응물 | Sulfur | HCID 5362487 | — |
| 반응물 | Potassium permanganate silicon dioxide | HCID 23697328 | — |
| 용매 | Ethanol | HCID 702 | — |
| 용매 | Water | HCID 962 | — |
| 용매 | Toluene | HCID 1140 | — |
| 용매 | Acetonitrile | HCID 6342 | — |
| 생성물 | 3-(1H-imidazol-2-yl)-2-methylpyridine | HCID 59198842 | — |
반응 단계
2-Methyl-3-pyridinecarbonitrile 1.05 g, ethylenediamine 5 mL and sulfur 71 mg were mixed, and stirred at 120° C. for 24 hours. Cooling it off to room temperature, toluene and water were added to effect phase separation. The aqueous layer was dried to solid under reduced pressure. Thus obtained crude product was mixed with potassium permanganate/silicon dioxide (carried at a ratio of 2.81 g:3.57 g) 6.38 g and acetonitrile 10 mL at room temperature, and stirred (inducing a rapid exothermic reaction). After the exotherm subsided and the reaction liquid was restored to room temperature, the liquid was diluted with 20 mL of ethanol and filtered through Celite. The solvent was distilled off and the residue was recrystallized from ethyl acetate/methanol (10:1) to provide 1.03 g of the title compound.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 특허 번호 | US08829000B2 |
|---|
| 출처 데이터셋 | uspto-grants-2014_09 |
|---|
| ORD ID | ord-c9acd577965d45f4ba22a52ca2776db2 |
|---|
| 출처 메모 | uspto-grants-2014_09 |
|---|