Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|
| Edukt | Water | HCID 962 | — |
| Edukt | Dabco | HCID 9237 | — |
| Edukt | N-methyl-2-pyrrolidone | HCID 13387 | — |
| Edukt | Dimethylthiocarbamoyl chloride | HCID 27871 | — |
| Edukt | 5-Bromo-2-methoxyphenol | HCID 142228 | — |
| Produkt | O-4-bromo-2-methoxyphenyl dimethylcarbamothioate | HCID 59339617 | — |
Reaktionsschritte
A mixture of 4-bromoguaiacol (2.05 g, 10.1 mmol) and 1,4-diazabicyclo(2.2.2)octane (1.42 g, 12.6 mmol) in NMP (24 mL) was heated at 50° C. to give a dark-yellow solution. A solution of dimethylthiocarbamoyl chloride (1.37 g, 11.1 mmol) in NMP (2 ml) was added dropwise to the previous solution over 1-2 min. Some precipitated has formed during the addition. The mixture was stirred at 50° C. for 3 h, and then water (25 ml) was added over 5 min at 50° C. The mixture was stirred overnight at r.t., and the precipitate was isolated by filtration, washed twice with water, and dried in vacuo at 50° C. to yield a pale creamed-coloured crystalline solid, 2.11 g (72%).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patentnummer | US07728030B2 |
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| Quelldatensatz | uspto-grants-2010_06 |
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| ORD ID | ord-22927637731c442b9632d5b40b43532b |
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| Quellennotiz | uspto-grants-2010_06 |
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