Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Dichloromethane → (4-Dimethylaminopiperidin-1-yl)(9H-xanthen-9-yl)methanone
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Dichloromethane | HCID 6344 | — |
| 반응물 | 1-Ethyl-3-(3'-dimethylaminopropyl)carbodiimide | HCID 15908 | — |
| 반응물 | Xanthene-9-carboxylic acid | HCID 65736 | — |
| 반응물 | 1-Hydroxybenzotriazole | HCID 75771 | — |
| 반응물 | Diisopropylethylamine | HCID 81531 | — |
| 반응물 | N,N-Dimethylpiperidin-4-amine | HCID 417391 | — |
| 생성물 | (4-Dimethylaminopiperidin-1-yl)(9H-xanthen-9-yl)methanone | HCID 59828537 | 90.4% |
반응 단계
To a stirred solution of 9H-xanthene-9-carboxylic acid (4.4 g, 19.4 mmol) in DCM (200 mL, 3 mol) was added dimethylpiperidin-4-yl-amine (2.5 g, 19.4 mmol). DIPEA (6.8 mL, 38.9 mmol) and HOBt (4.6 g, 34 mmol) were added to the mixture, followed by EDCI (4.5 g, 23.3 mmol). The mixture was stirred for 12 hours, then washed with water (300 mL), NaCl (sat.) (300 mL), dried over MgSO4 and then filtered. The solvent was removed under reduced pressure, and the crude material was purified via silica gel chromatography (10% MeOH/DCM w/1% NH3 (aq)) to yield the title compound (5.9 g).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US08492407B2 |
| 출처 데이터셋 | uspto-grants-2013_07 |
| ORD ID | ord-6135f0bb52af48d8b1055ba25220b62a |
| 출처 메모 | uspto-grants-2013_07 |