関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Dimethyl Sulfoxide | HCID 679 | — |
| 反応物 | N-Benzyl-N-methylethanolamine | HCID 66876 | — |
| 反応物 | Diisopropylethylamine | HCID 81531 | — |
| 反応物 | Sulfur trioxide-pyridine | HCID 168533 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 2-[Methyl(phenylmethyl)amino]acetaldehyde | HCID 20644698 | — |
反応手順
To a 3-necked 2-L flask was added N-benzyl-N-methylethanolamine (30.5 g, 0.182 mol), DCM (0.5 L), DIPEA (95 mL, 0.546 mol) and DMSO (41 mL, 0.728 mol). Using an ice bath, the mixture was cooled to about −10° C. and sulfur trioxide pyridine-complex (87 g, 0.546 mol) was added in 4 portions over 5 minute intervals. The reaction was stirred at −10° C. for 2 hours. Before removing the ice-bath, the reaction was quenched by adding water (0.5 L). The aqueous layer was separated and the organic layer was washed with water (0.5 L) and brine (0.5 L) and then dried over magnesium sulfate and filtered to provide the title compound which was used without further purification.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US08487107B2 |
|---|
| 出典データセット | uspto-grants-2013_07 |
|---|
| ORD ID | ord-e05f3d58ae1f430cbb111648208e408a |
|---|
| 出典メモ | uspto-grants-2013_07 |
|---|