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Water → 1-(4-chloropentyl)-5-methyl-2,4(1H,3H)-pyrimidinedione
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Thymine | HCID 1135 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 1-Bromo-4-chloropentane | HCID 15416791 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 1-(4-chloropentyl)-5-methyl-2,4(1H,3H)-pyrimidinedione | HCID 68693580 | — |
反応手順
A mixture of 5-methyl-2,4(1H,3H)-pyrimidinedione (thimine, 500 mg) and K2CO3 (548 g) in dry DMF (15 mL) was stirred for 1 hour at room temperature. 1-bromo-4-chloropentane (0.548 mL) was then added and the mixture was stirred at room temperature for 4 hours. Water was then added and the resulting mixture was extracted with dichloromethane. The aqueous phase was acidified to pH 7 with aqueous 2% HCl solution and extracted with DCM. The organic phases were dried and concentrated in vacuo. The crude product was purified by a silica SPE cartridge eluting with DCM/MeOH from 98/2 to 95/5 to give the title compound (100 mg).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07727988B2 |
| 出典データセット | uspto-grants-2010_06 |
| ORD ID | ord-37721b0f049b466395e868dac77cf5c5 |
| 出典メモ | uspto-grants-2010_06 |