反応式
NC(=O)c1ccc(Cl)nc1.NCc1ccccc1C(F)(F)F>CC(=O)O.CC(=O)O.CC(C)(C)[O-].COCCOC.[Na+].[Pd].c1ccc(P(c2ccccc2)c2ccc3ccccc3c2-c2c(P(c3ccccc3)c3ccccc3)ccc3ccccc23)cc1>NC(=O)c1ccc(NCc2ccccc2C(F)(F)F)nc1参加物
7
反応条件
- 温度
- 120 °C
実験手順
To a stirred solution of 6-chloronicotinamide (0.053 g, 0.34 mmol), 2,2'-bis(diphenylphosphino)-1,1'-binaphthyl (0.021 g, 0.03 mmol), sodium 2-methylpropan-2-olate (0.065 g, 0.68 mmol) and diacetoxypalladium (7.60 mg, 0.03 mmol) in DME (1 mL) was added (2-(trifluoromethyl)phenyl)methanamine (0.095 mL, 0.68 mmol). The reaction mixture was subjected to microwave irradiation for 4h at 120 C. Only traces of product was observed. The crude product was dissolved in DMSO (2 mL) and purified using Fractionlynx I, (Xbridge Prep C18 5µm OBD 19x150 mm column), with 5 to 95% acetonitrile in 0.2% ammonia at pH 10. 6-(2-(trifluoromethyl)benzylamino)nicotinamide: 1.45 mg (1.5 %)
出典と根拠
- ORDレコード
- ord-c7ac817750064edba47d3c6c786a7b69
- 出典データセット
- 750 AstraZeneca ELN dataset
- 元リンク
- 出典を表示
関連ノート
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