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Methane → Isopropyl 1,4,5,6-Tetrahydropyrimidine-5-carboxylate Hydrochloride
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Methane | HCID 297 | — |
| 反応物 | Isopropanol | HCID 3776 | — |
| 反応物 | Thionyl Chloride | HCID 24386 | — |
| 反応物 | 1,4,5,6-Tetrahydropyrimidine-5-carboxylic acid hydrochloride | HCID 70342184 | — |
| 生成物 | Isopropyl 1,4,5,6-Tetrahydropyrimidine-5-carboxylate Hydrochloride | HCID 20080421 | 84% |
反応手順
1,4,5,6-Tetrahydropyrimidine-5-carboxylic acid hydrochloride (1.0 g, 6.08 mmol) was suspended in 2-propanol (50 ml) and thionyl chloride (0.76 g, 6.39 mmol) was added dropwise. The resulting mixture was refluxed 24h. The pink solution was treated with charcoal and then reduced in volume to 15 ml by evaporating unreacted alcohol. By allowing the solution to stand overnight, white crystals (1.08 g, 84%) were obtained in three crops, mp 170° C. 300 MHz nmr confirmed product. Microanalysis calc.: C 46.49, H 7.26, N 13.56, found: C 46.49, H 7.25, N 13.64.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05403845 |
| 出典データセット | uspto-grants-1995_04 |
| ORD ID | ord-c2c5fed39ba44851add36118fd640225 |
| 出典メモ | uspto-grants-1995_04 |