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Methylamine → Ethyl 1,3-dimethyl-4-methylamino-1H-pyrazolo[3,4-b]pyridine-5-carboxylate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Methylamine | HCID 6329 | — |
| 反応物 | ethyl 4-chloro-1,3-dimethyl-1H-pyrazolo[3,4-b]pyridine-5-carboxylate | HCID 2736380 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | Ethyl 1,3-dimethyl-4-methylamino-1H-pyrazolo[3,4-b]pyridine-5-carboxylate | HCID 22322154 | 57.6% |
反応手順
A mixture of 1.268 g (5 mmol) of ethyl 4-chloro-1,3-dimethyl-1H-pyrazolo[3,4-b]pyridine-5-carboxylate and 7.5 ml (15 mmol) of methylamine in tetrahydrofuran (2.0 molar solution) was stirred at room temperature overnight and refluxed for 2 hours. The solvent was removed to give a white solid. The solid was dissolved in ethyl acetate and the solution washed with H2O, 1M NaHCO3, brine and dried (Na2SO4). The solvent was removed to give a white solid. Crystallization from ethyl acetate gave 0.715 g of white solid; Mass spectrum (ES) 249.2 (M+H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06946473B2 |
| 出典データセット | uspto-grants-2005_09 |
| ORD ID | ord-60dccb4e528f4eb9b5ed92a96baf4a23 |
| 出典メモ | uspto-grants-2005_09 |