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HRID 9911作成日:2026年10月26日

Dimethylformamide → 2-chloro-9-ethyl-6-(3-fluoro-phenyl-amino)-9H-purine

https://huagongshe.com/reaction/9911

反応式

関与物質

役割名称HCID仕込み量
反応物DimethylformamideHCID 6228—
反応物IodoethaneHCID 6340—
反応物Cesium carbonateHCID 10796—
反応物2-Chloro-6-(3-fluoro-phenyl-amino)-purineHCID 21988328—
溶媒Ethyl AcetateHCID 8857—
溶媒1,4-Dioxane--water (1/1)HCID 21886435—
生成物2-chloro-9-ethyl-6-(3-fluoro-phenyl-amino)-9H-purineHCID 21988319—

反応手順

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).

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US07091346B1
出典データセットuspto-grants-2006_08
ORD IDord-598185acff304cc3a86a995c03c157bb
出典メモuspto-grants-2006_08