関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | (Tetrahydrofuran-3-yl)methyl methanesulfonate | HCID 22273010 | — |
| 反応物 | HCID 178448879 | HCID 178448879 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | N2-Butyl-8-(methoxy)-9-(tetrahydro-3-furanylmethyl)-9H-Purine-2,6-diamine | HCID 57699650 | — |
反応手順
To a solution of N2-butyl-8-methoxy-9H-purine-2,6-diamine trifluoroacetic acid salt (3.89 g) in dry N,N-dimethylformamide (46 ml) at room temperature and under was added potassium carbonate (6.14 g) in one go. The reaction was heated to 60° C., under nitrogen, for 1.5 hours. A solution of tetrahydro-3-furanylmethyl methanesulfonate, Isomer 1 (2.2 g) in dry N,N-dimethylformamide (2 ml) was added via a Pasteur pipette and the reaction heated at 70° C. for 16 hours. The reaction was cooled to room temperature, diluted with ethyl acetate (100 ml) and washed with brine (20 ml). The organic layer was concentrated in vacuo. The product was purified by C18 reverse phase chromatography using water (0.1% formic acid)-acetonitrile (0.05% formic acid) as eluant (10-50%) to afford the title compound as a clear viscous oil (2.79 g).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07977344B2 |
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| 出典データセット | uspto-grants-2011_07 |
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| ORD ID | ord-183935e961134aa2b0a7ede45230c097 |
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| 出典メモ | uspto-grants-2011_07 |
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