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 | Carbamodithioic acid, N,N-dimethyl-, 2-oxopropyl ester | HCID 29494 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | 1-Acetylethylene dimethyldithiocarbamate | HCID 86734533 | — |
反応手順
A solution of acetonyl dimethyldithiocarbamate (3.6 grams, 0.020 mole), formaldehyde (1.6 grams of 37% aqueous solution, 0.020 mole), carbon disulfide (0.010 mole, 0.8 gram), and dimethylammonium dimethyldithiocarbamate (3.3 grams, 0.02 mole) in methanol (15 ml.) was stirred and heated at 39° - 43° C. for 160 minutes. The reaction mixture was then cooled in ice and the precipitated product was filtered off, washed with cold methanol, and dried in air. The yield of product melting at 104° - 106.5° C. (prior sintering) was 5.2 grams (84%). Repeated recrystallization from methylene chloride-methanol solution without heat gave the analytical sample of 1-acetylethylene dimethyldithiocarbamate melting at 105° - 107.5° C. (prior sintering). The structure was determined from the infrared spectrum and elemental analysis.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 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-482d10fbd6c1460299026acb215953a2 |
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| 出典メモ | uspto-grants-1977_07 |
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