化工社化工社 化学情報印刷レポート · 研究参考用
Sodium Hydroxide → 1,7,10-Trioxadispiro(2.2.4^(6).2^(3))dodecane
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | 1,4-Dioxaspiro[4.5]decan-8-one | HCID 567415 | — |
| 反応物 | Trimethylsulfonium methyl sulfate | HCID 2760871 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 1,7,10-Trioxadispiro(2.2.4^(6).2^(3))dodecane | HCID 12075953 | 93% |
反応手順
12.00 g (76.83 mmol, 1.0 equiv.) of 1,4 Cyclohexanedione ethylene ketal was added to 120 ml methylene chloride along with 18.8 g (99.88 mmol, 1.3 equiv.) of trimethyl sulfonium methyl sulfate. 40 ml 50% sodium hydroxide (NaOH) was added last and the reaction was refluxed for 24 hours. The methylene chloride was removed, 200 ml ether was added and the ether layer was washed with water. The organic layer was dried with sodium sulfate and concentrated down, leaving a yellow oil, 1,7,10-trioxa-dispiro[2.2.4.2]dodecane. (12.13 g, 93% yield). No further purification was necessary.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06664258B1 |
| 出典データセット | uspto-grants-2003_12 |
| ORD ID | ord-74e1ae7b45ae415898970a1391756682 |
| 出典メモ | uspto-grants-2003_12 |