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Stearoyl chloride → Octadecanoic acid 2-(2-aminoethoxy)ethyl ester hydrochloride
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Stearoyl chloride | HCID 8212 | — |
| 反応物 | HO-Peg-amine hcl | HCID 18764647 | — |
| 溶媒 | Acetone | HCID 180 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | Octadecanoic acid 2-(2-aminoethoxy)ethyl ester hydrochloride | HCID 85772808 | 40% |
反応手順
Stearoyl chloride (6.4 g; 21 mmol) (commercial product) was added dropwise in 5 min to a solution of 2-(2-aminoethoxy)ethanol hydrochloride (2.9 g; 20 mmol) in DMF (50 mL) at room temperature to afford a suspension. After 16 h, the suspension was diluted with acetone and the precipitated solid filtered and washed with acetone. The crude was crystallized from EtOAc; the solid was filtered, washed with EtOAc and dried under reduced pressure to give the desired compound (3.3 g; 8 mmol). Yield 40%. Acidic titer (0.1 N NaCH): 93%. K.F.: 1.06%. The 1H-NMR, 13C-NMR, MS and IR spectra were consistent with the structure.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06652834B2 |
| 出典データセット | uspto-grants-2003_11 |
| ORD ID | ord-dd7104a734f3465185cca07e169ffb5a |
| 出典メモ | uspto-grants-2003_11 |