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Diisopropylamine → Ethyl 2-benzylideneamino-2-ethylhexanoate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Diisopropylamine | HCID 7912 | — |
| 反応物 | Hexane | HCID 8058 | — |
| 反応物 | Butyl iodide | HCID 10962 | — |
| 反応物 | Ethyl 2-benzylideneaminobutyrate | HCID 10331026 | — |
| 反応物 | Butyllithium | HCID 178418339 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 溶媒 | Diethylether water | HCID 21584184 | — |
| 生成物 | Ethyl 2-benzylideneamino-2-ethylhexanoate | HCID 10107458 | 100% |
反応手順
A 1.6M solution of n-butyl lithium in hexane (33 mmoles, Aldrich) was added to a solution of diisopropylamine (40 mmoles) in THF (21 ml) at a temperature of 5°-10° C. When addition was complete, the mixture was added to a solution of the product from step (b) (30 mmoles) in THF (20 ml) at a temperature of 5°-10° C. When addition was complete, n-butyl iodide (40 mmoles) was added and the mixture allowed to warm to room temperature. After 20 hours, the mixture was poured into water/diethyl ether (1.1 L/0.5 L) and the organic layer separated, washed with brine (1.1 L), dried and evaporated in vacuo to give the desired product as an amber liquid (100% yield).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05859240 |
| 出典データセット | uspto-grants-1999_01 |
| ORD ID | ord-456d6594309a4628989b501e42d82b3f |
| 出典メモ | uspto-grants-1999_01 |