関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Formaldehyde | HCID 712 | — |
| 反応物 | Carbon Disulfide | HCID 6348 | — |
| 反応物 | Dimethyldithiocarbamic acid, dimethylamine | HCID 11728 | — |
| 反応物 | 2-Oxo-2-phenylethyl dimethylcarbamodithioate | HCID 238111 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | 1-Benzoylethylene dimethyldithiocarbamate | HCID 86734534 | — |
反応手順
A solution of phenacyl dimethyldithiocarbamate (12.0 grams, 0.050 mole), formaldehyde (4.1 grams of 37% aqueous solution, 0.050 mole), carbon disulfide (1.9 grams, 0.025 mole), and dimethylammonium dimethyldithiocarbamate (8.3 grams, 0.050 mole) in methanol (50 ml.) was stirred and heated at 38° - 40° C. for 2.5 hours. The reaction mixture was then cooled to 0° C. and the precipitated product was filtered off, washed with cold methanol and dried in air. The yield of product melting at 106° - 108.5° C. was 17.6 grams (94%). Repeated recrystallization from methylene chloride-methanol and acetone-2-propanol solution without heat gave pure 1-benzoylethylene dimethyldithiocarbamate melting at 106° - 109.5° C. The structure was determined from the infrared spectrum and elemental analysis.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US04038288 |
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| 出典データセット | uspto-grants-1977_07 |
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| ORD ID | ord-383aab3d8ca849bc8fcbc278467a3aba |
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| 出典メモ | uspto-grants-1977_07 |
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