Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
1,1'-Carbonyldiimidazole → 5-(6-chloro-4-(isopropylamino)pyridin-3-yl)-1,3,4-oxadiazol-2(3H)-one
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | 1,1'-Carbonyldiimidazole | HCID 68263 | — |
| 반응물 | 6-Chloro-4-(isopropylamino)nicotinohydrazide | HCID 89689668 | — |
| 용매 | Dimethylformamide | HCID 6228 | — |
| 생성물 | 5-(6-chloro-4-(isopropylamino)pyridin-3-yl)-1,3,4-oxadiazol-2(3H)-one | HCID 89690809 | — |
반응 단계
6-chloro-4-(isopropylamino)nicotinohydrazide (10) (800 mg, 3.5 mmol) was taken in DMF (4 mL). Added CDI (3.8 mmol, 1.1 equiv.) and stirred at room temperature for overnight. The reaction mass was concentrated under reduced pressure to remove excess of DMF. The residue was diluted using EtOAc, washed the EtOAc layer with water followed by brine solution. Collected the EtOAc layer, dried over Na2SO4, filtered and concentrated. The crude material obtained was taken to next step as such, without purification. LC/MS: Acquity BEH C18 2.1×50 mm, 1.8 micron; Solvent A=0.1% TFA in water; Solvent B=0.1% TFA in ACN; gradient 0-100% B over 2 min; retention time: 0.76 min; LCMS (ES-API), m/z 255.6 (M+H).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US09242975B2 |
| 출처 데이터셋 | uspto-grants-2016_01 |
| ORD ID | ord-b5f9b7339f1d48eab6d70d1c62750fa9 |
| 출처 메모 | uspto-grants-2016_01 |