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Diethylamine → Ethyl 6-((diethylamino)methyl)picolinate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Diethylamine | HCID 8021 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | Ethyl 6-(chloromethyl)pyridine-2-carboxylate | HCID 15614003 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | Ethyl 6-((diethylamino)methyl)picolinate | HCID 67125927 | 64% |
反応手順
To a suspension of ethyl 6-(chloromethyl)picolinate (200 mg, 1.00 mmol) and KI (166 mg, 1.00 mmol) in DMF was added N,N-diethyl amine (73 mg, 1.00 mmol) and K2CO3 (304 mg, 2.20 mmol). The reaction mixture was stirred at rt for 5 h. LC-MS indicated the presence of product. The solvent was evaporated under reduced pressure and the residue was partitioned between EtOAc (20 mL) and water (20 mL). The organic layer was washed with water (15 mL) and dried over Na2SO4. The solvent was evaporated under reduced pressure to give ethyl 6-((diethylamino)methyl)picolinate (150 mg, 64%) as an oil. LC-MS (ESI) m/z 237 (M+H)+.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US09296722B2 |
| 出典データセット | uspto-grants-2016_03 |
| ORD ID | ord-62e4d1b332844826bfe32f1ac5a90df1 |
| 出典メモ | uspto-grants-2016_03 |