Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|
| Edukt | Chlorine | HCID 24526 | — |
| Edukt | Triethyl orthoacetate | HCID 66221 | — |
| Lösungsmittel | Ethanol | HCID 702 | — |
| Produkt | 1,1,1-Trimethoxy-2-chloroethane | HCID 144702 | 90,9% |
Reaktionsschritte
A 1000 ml flask equipped with a stirrer and gas inlet tube was initially charged at 10° C. with a mixture of 648 g (4 mol) of 1,1,1-triethoxyethane and 70 g (approx. 11% by weight) of ethanol. Within 4 hours, 260 g (3.70 mol) of chlorine were introduced into the flask in gaseous form, and the internal temperature of the flask did not rise above 15° C. Once the entire amount of chlorine had been introduced into the flask, the mixture was worked-up by distillation. A distillation apparatus having approx. 5 theoretical plates was used to remove low boilers such as methanol and methyl acetate in the first stages at a reflux ratio of 5:1. In the main fraction, 520 g of 2-chloro-1,1,1 trimethoxyethane in a purity of >99.0% were obtained at a reflux ratio of 2:1. This amount of product corresponds to a yield of approx. 67%.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patentnummer | US06747176B2 |
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| Quelldatensatz | uspto-grants-2004_06 |
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| ORD ID | ord-b1cffe1cc2cb4f5788d33cc2b2601b95 |
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| Quellennotiz | uspto-grants-2004_06 |
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