関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Chlorine | HCID 24526 | — |
| 反応物 | Triethyl orthoacetate | HCID 66221 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | 1,1,1-Trimethoxy-2-chloroethane | HCID 144702 | 90.9% |
反応手順
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%.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06747176B2 |
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| 出典データセット | uspto-grants-2004_06 |
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| ORD ID | ord-b1cffe1cc2cb4f5788d33cc2b2601b95 |
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| 出典メモ | uspto-grants-2004_06 |
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