Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Methanol → 1-(4-Methylpyridin-3-yl)-3-(4-methylthieno[3,2-e]pyridin-2-yl)imidazolidin-2-one
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Methanol | HCID 887 | — |
| 반응물 | Potassium Carbonate | HCID 11430 | — |
| 반응물 | Methylboronic Acid | HCID 139377 | — |
| 반응물 | 1-(4-Chloro-thieno[3,2-c]pyridin-2-yl)-3-(4-methyl-pyridin-3-yl)-imidazolidin-2-one | HCID 49871870 | — |
| 촉매 | Tetrakis(triphenylphosphine)palladium | HCID 11979704 | — |
| 용매 | Chloroform | HCID 6212 | — |
| 생성물 | 1-(4-Methylpyridin-3-yl)-3-(4-methylthieno[3,2-e]pyridin-2-yl)imidazolidin-2-one | HCID 68782649 | 16.39% |
반응 단계
Tetrakis (triphenylphosphine) palladium (33 mg, 0.0288 mmol) was added to potassium carbonate (120 mg, 0.8649 mmol) previously purged with argon (30 minutes). The reaction mixture was purged with argon for 15 minutes, followed by the addition of 1-(4-chloro-thieno[3,2-c]pyridin-2-yl)-3-(4-methyl-pyridin-3-yl)-imidazolidin-2-one (98A: 100 mg, 0.2883 mmol) and methyl boronic acid (21 mg, 0.3459 mmol). The reaction mixture was heated to reflux for 6 hours. The reaction was monitored by TLC (10% MeOH in CHCl3). The reaction mixture was concentrated to afford the crude product. Purification by column chromatography on silica gel (3-4% MeOH in CHCl3), followed by preparative HPLC afforded 10 mg of the product (16.39% yield).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | USRE045173E1 |
| 출처 데이터셋 | uspto-grants-2014_09 |
| ORD ID | ord-d1ef7f24fe0c4034b7ba44cc299852fa |
| 출처 메모 | uspto-grants-2014_09 |