Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Dimethylformamide → 2-chloro-9-ethyl-6-(3-fluoro-phenyl-amino)-9H-purine
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Dimethylformamide | HCID 6228 | — |
| 반응물 | Iodoethane | HCID 6340 | — |
| 반응물 | Cesium carbonate | HCID 10796 | — |
| 반응물 | 2-Chloro-6-(3-fluoro-phenyl-amino)-purine | HCID 21988328 | — |
| 용매 | Ethyl Acetate | HCID 8857 | — |
| 용매 | 1,4-Dioxane--water (1/1) | HCID 21886435 | — |
| 생성물 | 2-chloro-9-ethyl-6-(3-fluoro-phenyl-amino)-9H-purine | HCID 21988319 | — |
반응 단계
1 g (3.47 mmol) of 2-chloro-6-(3-fluoro-phenyl-amino)-purine, 1.8 g (5.5 mmol) of caesium carbonate and 2.3 ml (27.8 mmol) of iodoethane are stirred in 14 ml of a dioxane/water mixture (4:3) and 12 ml of DMF at RT for 16 h. Thereafter, the reaction mixture is diluted with ethyl acetate and the organic phase is washed with water and dried over sodium sulfate. After removal of the solvent, the residue is chromatographed over silica gel (mobile phase: ethyl acetate/hexane=4:1) and 2-chloro-9-ethyl-6-(3-fluoro-phenyl-amino)-9H-purine is isolated; m.p. 136° C.; FAB-MS: (M+H)+=292; Rf=0.7 (CH2Cl2:methanol=9:1).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US07091346B1 |
| 출처 데이터셋 | uspto-grants-2006_08 |
| ORD ID | ord-598185acff304cc3a86a995c03c157bb |
| 출처 메모 | uspto-grants-2006_08 |