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Triethylamine → 3-[(5-bromo-2-chloro-pyrimidin-4-yl)-[(3,5-dimethoxyphenyl)methyl]amino]-N-methyl-propanamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | 5-Bromo-2,4-dichloropyrimidine | HCID 289973 | — |
| 反応物 | 3-[(3,5-dimethoxyphenyl)methylamino]-N-methyl-propanamide | HCID 61860673 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 3-[(5-bromo-2-chloro-pyrimidin-4-yl)-[(3,5-dimethoxyphenyl)methyl]amino]-N-methyl-propanamide | HCID 86617575 | 26.2% |
反応手順
3-[(3,5-dimethoxyphenyl)methylamino]-N-methyl-propanamide (Intermediate 98; 1 g, 3.96 mmol) was dissolved in DCM (10 mL) and triethylamine (0.68 mL, 4.36 mmol). 5-bromo-2,4-dichloropyrimidine (Aldrich; 993 mg, 4.36 mmol) was added and the mixture stirred at room temperature for 18 hours. The mixture was diluted with DCM and washed with water, brine, dried (MgSO4), filtered and evaporated to give a yellow gum which was purified on a 40 g ISCO companion eluting with 50-70% ethyl acetate in iso-hexane to give the title compound as a white solid (461 mg, 26%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07709471B2 |
| 出典データセット | uspto-grants-2010_05 |
| ORD ID | ord-70422d208bb048c3a2c8d05054ed0ab8 |
| 出典メモ | uspto-grants-2010_05 |