Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
1-Ethyl-3-(3'-dimethylaminopropyl)carbodiimide → HCID 58116841, 화합물
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | 1-Ethyl-3-(3'-dimethylaminopropyl)carbodiimide | HCID 15908 | — |
| 반응물 | Diisopropylethylamine | HCID 81531 | — |
| 반응물 | Piperazin-1-yl-pyrrolidin-1-yl-methanone | HCID 2760443 | — |
| 반응물 | 4-Bromocrotonic acid | HCID 6436411 | — |
| 반응물 | (3,4-Dichloro-phenyl)-(5,6,7,8-tetrahydro-9-thia-1,3,7-triaza-fluoren-4-yl)-amine | HCID 58116912 | — |
| 용매 | Water | HCID 962 | — |
| 용매 | Dichloromethane | HCID 6344 | — |
| 생성물 | HCID 58116841 | HCID 58116841 | 10% |
반응 단계
(2E)-4-Bromobut-2-enoic acid (106 mg, 0.64 mmol) and piperazin-1-yl(pyrrolidin-1-yl)methanone (125 mg, 0.68 mmol) were dissolved in DCM (5.0 mL), and DIPEA (111 mg, 0.85 mmol) was added. The mixture was stirred at rt for 2 h. Subsequently, the compound from Example 15A (150 mg, 0.43 mmol), DIPEA (55 mg, 0.43 mmol) and EDCI (82 mg, 0.43 mmol) were added. The reaction was stirred at 50° C. overnight. Then, water was added, and the mixture was extracted three times with DCM. The combined organic layers were dried over sodium sulfate. The solvent was removed in vacuo, and the residue was purified by preparative HPLC to yield 25 mg (10%) of the title compound.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US08524722B2 |
| 출처 데이터셋 | uspto-grants-2013_09 |
| ORD ID | ord-907f815ae1db4702b9a88f10da798df7 |
| 출처 메모 | uspto-grants-2013_09 |