関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Formaldehyde | HCID 712 | — |
| 反応物 | Morpholine | HCID 8083 | — |
| 反応物 | 1-Methyl-1H-pyrrole-2-carbaldehyde | HCID 14504 | — |
| 溶媒 | Acetic Acid | HCID 176 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 1-methyl-4-morpholin-4-ylmethyl-1H-pyrrole-2-carbaldehyde | HCID 86650822 | — |
| 生成物 | 1-methyl-5-morpholin-4-ylmethyl-1H-pyrrole-2-carbaldehyde | HCID 86650823 | — |
反応手順
To a solution of morpholine (130 mmoles) in acetic acid (60 ml) at 0° C. there are added 1-methyl-1H-pyrrole-2-carbaldehyde (110 mmoles) and formaldehyde (110 mmoles) 37% in water. The reaction mixture is stirred for 16 hours at 50° C. After evaporation to dryness, about 100 ml of 25% aqueous sodium hydroxide solution are added. After extraction with DCM, the organic phase is washed with water and with saturated aqueous NaCl solution, dried over sodium sulphate, filtered and evaporated to dryness. The residue is purified by flash chromatography on silica gel (SiO2; gradient AcOEt/MeOH) to yield the title products 1-methyl-4-morpholin-4-ylmethyl-1H-pyrrole-2-carbaldehyde and 1-methyl-5-morpholin-4-ylmethyl-1H-pyrrole-2-carbaldehyde in a ratio of 1/5.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US08541412B2 |
|---|
| 出典データセット | uspto-grants-2013_09 |
|---|
| ORD ID | ord-8838bff23f08415f88fe29d9cdc72eae |
|---|
| 出典メモ | uspto-grants-2013_09 |
|---|