Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Dichloromethane → 2-(6-(4-fluoro-phenoxy)-2-pyridin-2-yl-3H-benzimidazol-5-yl)-pyrrolidine-1-carboxamide
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Dichloromethane | HCID 6344 | — |
| 반응물 | 2-Dimethylaminopyridine | HCID 21885 | — |
| 반응물 | Trimethylsilyl isocyanate | HCID 70696 | — |
| 반응물 | 5-(4-fluoro-phenoxy)-2-pyridin-2-yl-6-pyrrolidin-2-yl-1H-benzimidazole | HCID 23145575 | — |
| 용매 | Water | HCID 962 | — |
| 생성물 | 2-(6-(4-fluoro-phenoxy)-2-pyridin-2-yl-3H-benzimidazol-5-yl)-pyrrolidine-1-carboxamide | HCID 23145349 | — |
반응 단계
2 mg of dimethylaminopyridine and 0.059 ml of trimethylsilyl isocyanate were added in order to a methylene chloride (1 ml) solution of 31.2 mg of 5-(4-fluoro-phenoxy)-2-pyridin-2-yl-6-pyrrolidin-2-yl-1H-benzimidazole obtained in Example 168, and the reaction liquid was stirred overnight at room temperature. Water was added to the reaction liquid, and extracted with ethyl acetate, and then washed with saturated saline. After dried and concentrated, the resulting residue was purified through reversed-phase middle-pressure liquid chromatography [ODS-AS-360-CC (by YMC), mobile phase: water-acetonitrile-0.1% trifluoroacetic acid] to obtain the entitled compound as a white solid.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US07728025B2 |
| 출처 데이터셋 | uspto-grants-2010_06 |
| ORD ID | ord-451f1694396b4bcab57ee743ed2e574c |
| 출처 메모 | uspto-grants-2010_06 |