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Sodium hydride → 2,6-Dichloro-9-((2-(trimethylsilyl)ethoxy)methyl)-9H-purine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | 2-Chloromethyl 2-(trimethylsilyl)ethyl ether | HCID 2724271 | — |
| 反応物 | 2,6-Dichloropurine | HCID 5324412 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 2,6-Dichloro-9-((2-(trimethylsilyl)ethoxy)methyl)-9H-purine | HCID 58285232 | — |
反応手順
945 mg of 2,6-dichloropurine, 15 ml of DMF (dimethylformamide) and 288 mg of NaH are mixed and left at ambient temperature for 2 hours. 1.06 ml of 2-chloromethoxyethyltrimethylsilane are then added. The mixture is stirred for 18 hours at ambient temperature. The DMF is evaporated off. The product is taken up in methylene chloride. Washing is carried out with a saturated sodium bicarbonate solution and then once with H2O and, finally, with a saturated NaCl solution. Drying over Na2SO4 and evaporation to dryness are carried out. Purification is carried out by chromatography on silica with a CHCl3-AcOEt: 5-5 mixture for eluent. 876 mg of expected product are obtained, in the form of a yellow-colored oil.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07476670B2 |
| 出典データセット | uspto-grants-2009_01 |
| ORD ID | ord-9dae688878cc4cd98e06386b3760b190 |
| 出典メモ | uspto-grants-2009_01 |