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Ethyl vinyl ether → 2-Methyl-5-hydroxymethyl-5-nitro-1,3-dioxane
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Ethyl vinyl ether | HCID 8023 | — |
| 反応物 | Tris(hydroxymethyl)nitromethane | HCID 31337 | — |
| 触媒 | Hydrochloric Acid | HCID 313 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 生成物 | 2-Methyl-5-hydroxymethyl-5-nitro-1,3-dioxane | HCID 15670910 | 86% |
反応手順
Following the procedure 2(A) described in this application, to a 100 ml round bottom flask equipped with a stir bar and reflux condenser topped with a nitrogen inlet was added 5 g (0.03 mol) tris(hydroxymethyl)nitromethane, 2.86 g (0.04 mol) ethylvinyl ether, 50 ml acetonitrile and 5 drops concentrated HCl. The reaction was heated to 35°-40° C. for 4 hours. After cooling to room temperature the volatiles were removed to give the product, 2-methyl-5-hydroxymethyl-5-nitro-1,3-dioxane, in 86% yield. 1H NMR in CD3OD confirmed the structure.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04978793 |
| 出典データセット | uspto-grants-1990_12 |
| ORD ID | ord-8261094aa39048659cc3d9f4fdbfe303 |
| 出典メモ | uspto-grants-1990_12 |