化工社化工社 化学情報印刷レポート · 研究参考用
Iodoethane → 3-ethyl-8-chloro-7-(2-propen-1-yl)-3,7-dihydro-1H-purine-2,6-dione
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Iodoethane | HCID 6340 | — |
| 反応物 | Sodium Carbonate | HCID 10340 | — |
| 反応物 | 7-Allyl-8-chloro-1H-purine-2,6(3H,7H)-dione | HCID 59299532 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 3-ethyl-8-chloro-7-(2-propen-1-yl)-3,7-dihydro-1H-purine-2,6-dione | HCID 59395639 | 75% |
反応手順
A solution of 8-chloro-7-(2-propen-1-yl)-3,7-dihydro-1H-purine-2,6-dione (10 g, 0.044 mol) in anhydrous DMF (100 ml) was treated with iodoethane (5.4 ml, 0.068 mol) and Na2CO3 (4.9 g, 0.046 mol). The reaction mixture was left to stir at rt under nitrogen for 2 days. Iodoethane (0.35 ml, 0.0044 mol) was added and the mixture was left to stir at rt for 1 day. The mixture was partitioned between EtOAc and 2M HCl. The organic layer was separated, washed sequentially with saturated sodium sulphite solution and brine, dried (MgSO4) and concentrated. The crude solid was washed with Et2O to give the title compound as a white solid (8.37 g, 75%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08143264B2 |
| 出典データセット | uspto-grants-2012_03 |
| ORD ID | ord-9d157e1df8794d71acbde4ab2fe74732 |
| 出典メモ | uspto-grants-2012_03 |