Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Cesium carbonate → 5-Chloro-2-methoxy-N-(2-(1-(3-cyclohexylthioureidosulfonyl)piperidin-4-yl)ethyl)benzamide
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Cesium carbonate | HCID 10796 | — |
| 반응물 | Cyclohexyl isothiocyanate | HCID 14289 | — |
| 반응물 | 4-(2-(5-Chloro-2-methoxybenzamido)ethyl)piperidine-1-sulfonamide | HCID 12282030 | — |
| 용매 | N-methyl-2-pyrrolidone | HCID 13387 | — |
| 생성물 | 5-Chloro-2-methoxy-N-(2-(1-(3-cyclohexylthioureidosulfonyl)piperidin-4-yl)ethyl)benzamide | HCID 59660712 | 45% |
반응 단계
376 mg (1 mmol) of 4-(2-(5-chloro-2-methoxybenzamido)ethyl)piperidine-1-sulfonamide and 652 mg (2.0 mmol) of cesium carbonate were heated in 5 ml of N-methyl-2-pyrrolidone with 0.3 ml (2 mmol) of cyclohexyl isothiocyanate at 80° C. for 10 minutes. The reaction mixture was poured onto ice/2 M hydrochloric acid, and the precipitated solid was filtered off with suction, washed with water until neutral, dissolved in methanol, filtered after addition of activated carbon and crystallized using diethyl ether. 230 mg (45%) of the title compound were obtained as a colorless solid.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US08586612B2 |
| 출처 데이터셋 | uspto-grants-2013_11 |
| ORD ID | ord-f9818bdd00444776a8546114a0618c35 |
| 출처 메모 | uspto-grants-2013_11 |