Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Isopropyl iodide → 2-chloro-9-isopropyl-6-(4-fluoro-phenyl-amino)-9H-purine
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Isopropyl iodide | HCID 6362 | — |
| 반응물 | Cesium carbonate | HCID 10796 | — |
| 반응물 | 1,4-Dioxane | HCID 31275 | — |
| 반응물 | 2-Chloro-6-(4-fluoro-phenyl-amino)-purine | HCID 21988193 | — |
| 용매 | Water | HCID 962 | — |
| 용매 | Dimethylformamide | HCID 6228 | — |
| 용매 | Ethyl Acetate | HCID 8857 | — |
| 생성물 | 2-chloro-9-isopropyl-6-(4-fluoro-phenyl-amino)-9H-purine | HCID 21988246 | — |
반응 단계
A mixture comprising 1 g (3.3 mmol) of 2-chloro-6-(4-fluoro-phenyl-amino)-purine, 2.1 g (6.6 mmol) of caesium carbonate and 2 ml of isopropyl iodide is stirred in 32 ml of a mixture comprising dioxane, water and DMF in a ratio of 2:3:7 at 100° C. for 20 h. Thereafter, the reaction mixture is diluted with ethyl acetate and the organic phase is washed with water. After drying over sodium sulfate and removal of the solvent, the residue is chromatographed over silica gel (mobile phase: ethyl acetate:hexane=4:1). On concentration, 2-chloro-9-isopropyl-6-(4-fluoro-phenyl-amino)-9H-purine is obtained as a crystalline compound. m.p. 154° C.; FAB-MS: (M+H)+=306; Rf=0.2 (ethyl acetate:hexane=4:1).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US07091346B1 |
| 출처 데이터셋 | uspto-grants-2006_08 |
| ORD ID | ord-aafe9cd2ac154742ae3af14c87c79dc2 |
| 출처 메모 | uspto-grants-2006_08 |