関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Nitrogen | HCID 947 | — |
| 反応物 | Potassium Hydroxide | HCID 14797 | — |
| 反応物 | N,N-bis(2-hydroxyethyl)-16-hydroxyhexadecanamide | HCID 19694613 | — |
| 反応物 | Aluminium lithium hydride | HCID 21226445 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 16-[N,N-bis(2-hydroxyethyl)amino]-1-hexadecanol | HCID 22015146 | 62% |
反応手順
A 500-ml flask equipped with a stirrer and reflux condenser was charged with 3.01 g (79.3 mmol) of LiAlH4 and 200 ml of tetrahydrofuran. While stirring the mixture at room temperature in an N2 atmosphere, 5.00 g (13.9 mmol) of N,N-bis(2-hydroxyethyl)-16-hydroxyhexadecanamide were added, followed by stirring at 65° C. for 18 hours. After cooling the reaction mixture to room temperature, 15 g of 3% aqueous KOH were added, and a salt deposited was separated by filtration. The solvent was then distilled off under reduced pressure, and the resultant residue was purified by column chromatography on silica gel, thereby obtaining 2.98 g (yield: 62%) of the title compound (IId-3).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US05723497 |
|---|
| 出典データセット | uspto-grants-1998_03 |
|---|
| ORD ID | ord-f7c05078e24046a8887d238bff8b0c4f |
|---|
| 出典メモ | uspto-grants-1998_03 |
|---|