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Methyl iodide → HCID 178503551、化合物
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Methyl iodide | HCID 6328 | — |
| 反応物 | Potassium Hydroxide | HCID 14797 | — |
| 反応物 | 2-Thiothymine | HCID 720471 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | HCID 178503551 | HCID 178503551 | 71.9% |
反応手順
5-methyl-2-thiouracil (2 g, 98%, 13.78 mmol, 1 eq) and KOH, 85%, (1.05 eq, 995 mg) were suspended in 25 ml of absolute ethanol and the mixture was stirred for 1 hour at room temperature. In the suspension was then added MeI (1.05 eq, 905 μl) dropwise and the suspension was heated at 65° C. (temperature on display of heating device) for 2 hours. Solvent was then evaporated. In the rest was added 100 ml of water and using ultrasound was suspended. The obtained precipitate was collected by filtration, it was dried and obtained was 5-methyl-2-methylsulfanyl-1H-pyrimidin-4-one (1.7 g, yield=71.9%, purity=93%) in form of a white powder. MS: [M+H]+=157.08 1H NMR (300 MHz; DMSO-d6) δ/ppm 1.90 (s, 3H), 2.50 (s, 3H), 7.78 (s, 1H)
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08637536B2 |
| 出典データセット | uspto-grants-2014_01 |
| ORD ID | ord-552263b096a04605a0fd7ee7332b43b7 |
| 出典メモ | uspto-grants-2014_01 |