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Water → 4-chloro-2-(N-(2-morpholin-4-ylethyl)carbamoyl)pyridine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | 2-Morpholinoethylamine | HCID 408285 | — |
| 反応物 | Methyl 4-chloropyridine-2-carboxylate--hydrogen chloride (1/1) | HCID 16655470 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 4-chloro-2-(N-(2-morpholin-4-ylethyl)carbamoyl)pyridine | HCID 23614579 | 95.4% |
反応手順
To a solution of methyl 4-chloropyridine-2-carboxylate HCl salt (Method A2, Step 2; 1.01 g, 4.86 mmol) in THF (20 mL) was added 4-(2-aminoethyl)morpholine (2.55 mL, 19.4 mmol) dropwise and the resulting solution was heated at the reflux temp. for 20 h, cooled to room temp., and treated with water (50 mL). The resulting mixture was extracted with EtOAc (50 mL). The organic layer was dried (MgSO4) and concentrated under reduced pressure to afford 4-chloro-2-(N-(2-morpholin-4-ylethyl)carbamoyl)pyridine as a yellow oil (1.25 g, 95%): TLC (10% MeOH/90% EtOAc) Rf 0.50.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08841330B2 |
| 出典データセット | uspto-grants-2014_09 |
| ORD ID | ord-ca6a6a4905ed4e3996dd133866f1f1e6 |
| 出典メモ | uspto-grants-2014_09 |