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Potassium Carbonate → 1-(4-Hydroxybutyl)-6-phenylthiothymine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 5-Methyl-6-phenyl-2-sulfanylidene-1,2,3,4-tetrahydropyrimidin-4-one | HCID 18671027 | — |
| 反応物 | 4-(t-Butyldimethylsiloxy)-butyl-p-toluenesulphonate | HCID 86749059 | — |
| 溶媒 | Dimethyl Sulfoxide | HCID 679 | — |
| 生成物 | 1-(4-Hydroxybutyl)-6-phenylthiothymine | HCID 54179830 | 4.1% |
反応手順
To 2 ml of dimethyl sulfoxide, 468 mg (2.0 mmol) of 6-phenylthiothymine, 358 mg (1.0 mmol) of 4-(t-butyldimethylsiloxy)-butyl-p-toluenesulphonate and 276 mg (2.0 mmol) of potassium carbonate were added and heated to react for 4 hours at 80° C. The reaction mixture was concentrated under reduced pressure, added with methanol and filtered. The filtrate was concentrated under reduced pressure, added with 20 ml of tetrahydrofuran and 1 ml of 1N hydrochloric acid and stirred for 90 minutes. The reaction mixture was concentrated under reduced pressure and adsorbed on a silica gel column and eluted with 2% methanol/chloroform. The eluate was concentrated and crystallized from acetone/hexane to obtain 12.0 mg of the target compound (Yield: 4%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05461060 |
| 出典データセット | uspto-grants-1995_10 |
| ORD ID | ord-8d8f8d9bad8f486387d7e1d7e75296f9 |
| 出典メモ | uspto-grants-1995_10 |