Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
1-Ethyl-3-(3'-dimethylaminopropyl)carbodiimide → 1-(tert-Butoxycarbonyl)-4-[{N-(9-fluorenylmethyloxycarbonyl)glycyl}aminomethyl]piperidine
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | 1-Ethyl-3-(3'-dimethylaminopropyl)carbodiimide | HCID 15908 | — |
| 반응물 | 1-Hydroxybenzotriazole | HCID 75771 | — |
| 반응물 | Fmoc-Gly-OH | HCID 93124 | — |
| 반응물 | 1-Boc-4-(aminomethyl)piperidine | HCID 736817 | — |
| 용매 | Dichloromethane | HCID 6344 | — |
| 용매 | Triethylamine | HCID 8471 | — |
| 생성물 | 1-(tert-Butoxycarbonyl)-4-[{N-(9-fluorenylmethyloxycarbonyl)glycyl}aminomethyl]piperidine | HCID 54127009 | 44% |
반응 단계
Triethylamine (3.51 g), N-(9-fluorenylmethyloxycarbonyl)glycine (7.93 g, 26.7 mmol), EDCI (3.80 g) and HOBt (4.33 g) were added to a dichloromethane (150 mL) solution of 4-(aminomethyl)-1-(tert-butoxycarbonyl)piperidine (5.72 g). The resulting reaction mixture was stirred at room temperature for 18 hours, then washed with water (100 mL×3) and brine (100 mL×2), dried over anhydrous sodium sulfate, concentrated and recrystallized from acetonitrile/methanol (150 mL/1 mL) at 0° C. to provide 1-(tert-butoxycarbonyl)-4-[[N-(9-fluorenylmethyloxycarbonyl)glycyl]aminomethyl]piperidine (5.75 g, 44%) as an off-white crystal.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US07390830B1 |
| 출처 데이터셋 | uspto-grants-2008_06 |
| ORD ID | ord-664513ffdb3d42019888ccb8997ce83a |
| 출처 메모 | uspto-grants-2008_06 |