Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|
| Edukt | Formaldehyde | HCID 712 | — |
| Edukt | Carbon Disulfide | HCID 6348 | — |
| Edukt | Dimethyldithiocarbamic acid, dimethylamine | HCID 11728 | — |
| Edukt | 2-Oxo-2-phenylethyl dimethylcarbamodithioate | HCID 238111 | — |
| Lösungsmittel | Methanol | HCID 887 | — |
| Produkt | 1-Benzoylethylene dimethyldithiocarbamate | HCID 86734534 | — |
Reaktionsschritte
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° C.-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° C.-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° C.-109.5° C. The structure was determined from the infrared spectrum and elemental analysis.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patentnummer | US04011230 |
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| Quelldatensatz | uspto-grants-1977_03 |
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| ORD ID | ord-c229064febd34a56ba134c21af52d765 |
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| Quellennotiz | uspto-grants-1977_03 |
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