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Hydrochloric Acid → 1,4,5,6-Tetrahydropyrimidine-5-carboxylic acid hydrochloride
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Pyrimidine-5-carboxylic acid | HCID 78346 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 1,4,5,6-Tetrahydropyrimidine-5-carboxylic acid hydrochloride | HCID 70342184 | 92.8% |
反応手順
Pyrimidine-5-carboxylic acid (5.0 g, 40 mmol) was suspended in a mixture of 150 ml water and concentrated hydrochloric acid (4.0 g, 40.5 mmol). The mixture was hydrogenated at 26 psig over 1.0 g Pd-on-carbon 10% in a Parr hydrogenator for 3h. The suspension was filtered and the filter rinsed twice with hot water (20 ml). The filtrate was evaporated in vacuo to give 6.11 g yellow oil (92%). The oil was crystallized from anhydrous methanol/tetrahydrofuran (THF) to give 5.77 g (87%) white crystals in two crops. 300 MHz nmr indicated product.
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-087bc02165fc4420a67f9622822fc2f7 |
| 出典メモ | uspto-grants-1995_04 |