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Potassium Carbonate → 2-Amino-6,8-dichloro-9-(2-(2,2-dimethyl-1,3-dioxan-5-yl)ethyl)purine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 1,3-Dioxane, 5-(2-bromoethyl)-2,2-dimethyl- | HCID 178988 | — |
| 反応物 | 6,8-Dichloro-9H-purin-2-amine | HCID 5464677 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 2-Amino-6,8-dichloro-9-(2-(2,2-dimethyl-1,3-dioxan-5-yl)ethyl)purine | HCID 19883991 | 44.6% |
反応手順
A mixture of 2-amino-6,8-dichloropurine (0.82 g), 5-bromoethyl-2,2-dimethyl-1,3-dioxan (0.9 g) and anhydrous potassium carbonate (0.83 g) in N,N-dimethylformamide (20 ml) was stirred at room temperature for 18 hours under dry nitrogen. The mixture was then filtered and the filtrate evaporated. The residue was purified by column chromatography on silica (100 g) [eluent 2% methanol-dichloromethane] to give 2-amino-6,8-dichloro-9-(2-(2,2-dimethyl-1,3-dioxan-5-yl)ethyl)purine (t.l.c. r.f. 0.50, 5% methanol-dichloromethane) as a pale solid (0.62 g, 45%). Recrystallisation from diethyl ether gave an off-white solid m.p. 149°-150° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05138057 |
| 出典データセット | uspto-grants-1992_08 |
| ORD ID | ord-a403aacc28a742d09c1c39cdb24ddfc7 |
| 出典メモ | uspto-grants-1992_08 |