化工社化工社 化学情報印刷レポート · 研究参考用
Water → 1-(4-chlorobutyl)-5-methylpyrimidine-2,4(1H,3H)-dione
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-chlorobutane | HCID 81364 | — |
| 溶媒 | Dimethyl Sulfoxide | HCID 679 | — |
| 生成物 | 1-(4-chlorobutyl)-5-methylpyrimidine-2,4(1H,3H)-dione | HCID 59337587 | — |
反応手順
A mixture of 5-methyl-2,4(1H,3H)-pyrimidinedione (thimine, 500 mg, commercially available from Aldrich) and K2CO3 (546 mg) in dry DMSO (15 mL) was stirred for 1 hour at room temperature. 1-bromo-4-chlorobutane (0.46 mL) was then added and the mixture was stirred at room temperature for 20 hours. Water was then added and the resulting mixture was extracted with EtAcO. The aqueous phase was acidified to pH 7 with aqueous 2% HCl solution and extracted with DCM. The organic phases were washed with brine, dried over Na2SO4 and concentrated in vacuo. The crude product was purified by a silica SPE cartridge (25 g) eluting with toluene/acetone from 95/5 to 75/25 to give the title compound as a colourless oil (250 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-41e3223279b340a3bb76d5a9cf5a22f9 |
| 出典メモ | uspto-grants-2010_06 |