関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Benzyl Alcohol | HCID 244 | — |
| 反応物 | Diethyl Ether | HCID 3283 | — |
| 反応物 | Thionyl Chloride | HCID 24386 | — |
| 反応物 | 1,4,5,6-Tetrahydropyrimidine-5-carboxylic acid hydrochloride | HCID 70342184 | — |
| 生成物 | Benzyl 1,4,5,6-Tetrahydropyrimidine-5-carboxylate Hydrochloride | HCID 20080426 | 76% |
反応手順
1,4,5,6-Tetrahydropyrimidine-5-carboxylic acid hydrochloride (1.0 g, 6.1 mmol) was suspended in dry benzyl alcohol (20 ml). To the mixture was added thionyl chloride (0.76 g, 6.39 mmol) and the resulting mixture was heated in an oil bath at 80° C. for 24h. The clear solution was poured to anhydrous ethyl ether (100 ml) to induce precipitation. The white solids were collected and crystallized from methanol/THF to give 1.18 g (76%) of product (mp 113°-114° C.). 300 MHz nmr indicated the product. Microanalysis calc.: C 56.58, H 5.89, N 11.00; found: C 56.34, H 6.03, N 11.19.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05403845 |
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| 出典データセット | uspto-grants-1995_04 |
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| ORD ID | ord-96504962717b40cf9c33794bd881f6c9 |
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| 出典メモ | uspto-grants-1995_04 |
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