関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Isopropanol | HCID 3776 | — |
| 反応物 | Ethyl 2-((dimethylamino)methyl)thiazole-4-carboxylate | HCID 2039211 | — |
| 反応物 | Sodium borohydride | HCID 4311764 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | (2-Dimethylaminomethyl-thiazol-4-yl)-methanol hydrochloride | HCID 13121938 | — |
反応手順
Alternatively, a mixture of 2.14 g of ethyl 2-dimethylaminomethyl-4-thiazolecarboxylate and 0.38 g of sodium borohydride in 20 ml. of isopropanol was heated with stirring at reflux temperature for about 14 hours. The reaction mixture was cooled, and 2 ml. of water were added carefully followed by 4 ml. of 5N aqueous hydrochloric acid. The volatile constituents were removed by evaporation. Methanol (10 ml.) was added and the mixture heated to refluxing temperature for about one hour. Methanol was removed by evaporation and the residual solids digested in 10 ml. of isopropanol on the steam bath. The isopropanol solution was separated by decantation and the solids reextracted with 10 m. of isopropanol. The isopropanol solutions and extracts were combined and the combined solution filtered while hot to remove insoluble material. The filtrate was chilled and a crystalline solid appeared which separated and was recovered by filtration. Recrystallization of the filter cake from isopropanol gave 1.73 g of 2-dimethylaminomethyl-4-thiazolemethanol hydrochloride melting at 153°-154° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04468399 |
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| 出典データセット | uspto-grants-1984_08 |
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| ORD ID | ord-52dc833f21ec475daa27250ab564d894 |
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| 出典メモ | uspto-grants-1984_08 |
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