関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Trifluoroacetic acid | HCID 6422 | — |
| 反応物 | 2,2-Bis(trifluoromethyl)-4-hydroxymethyl-1,3-dioxolane | HCID 21997103 | — |
| 反応物 | HCID 178418852 | HCID 178418852 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 2,2-Bis(trifluoromethyl)-4-carbamoyloxymethyl-1,3-dioxolane | HCID 21395794 | — |
反応手順
A mixture of 15 grams of 2,2-bis(trifluoromethyl)-4-hydroxymethyl-1,3-dioxolane (0.0625 mols), 8.12 grams NaOCN (0.125 mols), and 75 ml methylene dichloride is stirred at 25°-35° C. while 14.3 grams trifluoroacetic acid is added dropwise. The mixture is stirred for 16 hours at 40° C. The product is filtered and the filter cake washed with methylene dichloride. The filtrate is washed with water and dried over Na2SO4 prior to vacuum-stripping. The reaction product is recrystallized from 1 part benzene to yield 2,2-bis(trifluoromethyl)-4-carbamoyloxymethyl-1,3-dioxolane (m.p. 52°-54° C.)
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US03996376 |
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| 出典データセット | uspto-grants-1976_12 |
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| ORD ID | ord-92caa2051e0144a3b0e069b9145a2ab9 |
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| 出典メモ | uspto-grants-1976_12 |
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