化工社化工社 化学情報印刷レポート · 研究参考用
Ethylene Glycol → 1,5-Dioxa-9-azaspiro[5.5]undecane, 8,8,10,10-tetramethyl-
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Ethylene Glycol | HCID 174 | — |
| 反応物 | Water | HCID 962 | — |
| 反応物 | Phosphoric Acid | HCID 1004 | — |
| 反応物 | Toluene | HCID 1140 | — |
| 反応物 | 2,2,6,6-Tetramethyl-4-piperidone | HCID 13220 | — |
| 生成物 | 1,5-Dioxa-9-azaspiro[5.5]undecane, 8,8,10,10-tetramethyl- | HCID 11961786 | — |
反応手順
Use of Phosphoric Acid 77 g of triacetonamine were initially charged in 240 g of toluene together with 47 g of ethylene glycol. Subsequently, sufficient phosphoric acid (63 g) was added that the reaction mixture showed an acidic pH (≦2) when tested with a moistened indicator paper. The reaction mixture was heated to reflux temperature and water of reaction formed was removed on a water separator. After approx. 3 hours, there was less than 10% of the desired product according to the gas chromatogram. Instead, a plurality of secondary components had formed which were not investigated further.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07390930B2 |
| 出典データセット | uspto-grants-2008_06 |
| ORD ID | ord-7875deca30664fefb1e356d47aae5457 |
| 出典メモ | uspto-grants-2008_06 |