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Methyl Isocyanate → 2-oxo-4,5,5-trimethyl-3-thiazoline-O-(methylcarbamoyl)-oxime
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Methyl Isocyanate | HCID 12228 | — |
| 反応物 | 2-Oxo-4,5,5-trimethyl-3-thiazoline oxime | HCID 85997244 | — |
| 触媒 | Triethylamine | HCID 8471 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 2-oxo-4,5,5-trimethyl-3-thiazoline-O-(methylcarbamoyl)-oxime | HCID 86737551 | — |
反応手順
15.8 g (0.1 mol) of 2-oxo-4,5,5-trimethyl-3-thiazoline-oxime and 8.5 g. (0.15 mol) of methyl isocyanate were dissolved in 100 ml. of anhydrous dichloromethane. After a few drops of triethylamine were added to this solution, the mixture warmed to 40°-45° C. The mixture was warmed to 50°-60° C. for a short time and then the solvent was distilled off under vacuum. The residue was dissolved in 50 ml. of hot ethyl acetate, treated with carbon and filtered. The hot filtrate was concentrated to 20-30 ml. and treated with 20-30 ml. of hexane. The precipitated crystals were filtered off under vacuum, washed with ether and dried to yield 2-oxo-4,5,5-trimethyl-3-thiazoline-O-(methylcarbamoyl)-oxime, m.p. 123°-125° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04255436 |
| 出典データセット | uspto-grants-1981_03 |
| ORD ID | ord-9d6fd169d45f4e3eab23bc59a7840168 |
| 出典メモ | uspto-grants-1981_03 |