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Acetonitrile → 8-Octyl-1,4-dioxa-8-azaspiro[4.5]decane
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Acetonitrile | HCID 6342 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 1-Iodooctane | HCID 12380 | — |
| 反応物 | 1,4-Dioxa-8-azaspiro(4.5)decane | HCID 67435 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 8-Octyl-1,4-dioxa-8-azaspiro[4.5]decane | HCID 21249280 | 90% |
反応手順
To a mixture of 15 g (0.105 mol) of 1,4-dioxa-8-azaspiro[4.5]decane, 15.93 g (0.115 mol) of K2CO3, and 100 ml of acetonitrile is added dropwise 18.92 ml (0.105 mol) of iodooctane. The mixture is stirred overnight at room temperature and then at 65° C. for 2 hours. After cooling, the mixture was diluted with water and extracted with methylene chloride. The combined extracts are washed with brine, dried over Na2SO4, and concentrated in vacuo. The residue is triturated with ether and filtered. The filtrate is concentrated in vacuo to yield 24.04 g (90%) of title compound as a clear oil: IR (neat) 2925 and 1094 cm-1 ; NMR (CDCl3) δ3.97 (s, 4H), 2.56 (br, 4H), 2.38 (m, 2H), 1.78 (m, 4H), 1.51 (br, 2H), 1.28 (s, 10H), 0.89 (m, 3H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04816464 |
| 出典データセット | uspto-grants-1989_03 |
| ORD ID | ord-1304b6314bb14c6dbf27df954ac43158 |
| 出典メモ | uspto-grants-1989_03 |