참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Actarit | HCID 2018 | — |
| 반응물 | Dimethylformamide | HCID 6228 | — |
| 반응물 | 1,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochloride | HCID 2723939 | — |
| 반응물 | t-Butoxycarbonyl-aminopropanol | HCID 23149331 | — |
| 촉매 | 4-(Dimethylamino)pyridine | HCID 14284 | — |
| 용매 | Dichloromethane | HCID 6344 | — |
| 용매 | Ethyl Acetate | HCID 8857 | — |
| 생성물 | Boc-aminopropanol actarit | HCID 86623043 | 83% |
반응 단계
In 2 ml of dichloromethane, 123.1 mg (0.703 mmol) of the Boc-aminopropanol obtained in Reference Example 1 was dissolved, and then a DMF solution (1 ml) of 136.0 mg (0.704 mmol) of actarit was added thereto, and 17.1 mg (0.140 mmol) of DMAP and 175.4 mg (0.915 mmol) of WSCI.HCl were added thereto in this order under ice-cooling, followed by stirring overnight while gradually returning to room temperature. Ethyl acetate was added thereto, followed by separation by washing with 5% aqueous citric acid solution, 5% aqueous sodium hydrogen carbonate solution and saturated brine consecutively. After dehydration drying with sodium sulfate, ethyl acetate was evaporated under reduced pressure. The precipitate was purified by silica gel column chromatography to give 203.1 mg (83%) of the titled compound. The structure was identified by 1H-NMR.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 특허 번호 | US07879817B2 |
|---|
| 출처 데이터셋 | uspto-grants-2011_02 |
|---|
| ORD ID | ord-31cb5099ca0740c893807ef3f604837f |
|---|
| 출처 메모 | uspto-grants-2011_02 |
|---|
