反応式
C[C@@H]1CNCCN1.Fc1ccc(Br)c(C(F)(F)F)c1>CC(C)(C)[O-].Cc1ccccc1.O=C(/C=C/c1ccccc1)/C=C/c1ccccc1.O=C(/C=C/c1ccccc1)/C=C/c1ccccc1.O=C(/C=C/c1ccccc1)/C=C/c1ccccc1.[Na+].[Pd].[Pd].c1ccc(P(c2ccccc2)c2ccc3ccccc3c2-c2c(P(c3ccccc3)c3ccccc3)ccc3ccccc23)cc1>C[C@@H]1CN(c2ccc(F)cc2C(F)(F)F)CCN1参加物
反応物 2
生成物 1
試薬・触媒・溶媒 4
反応条件
- 温度
- 100 °C
実験手順
1-bromo-4-fluoro-2-(trifluoromethyl)benzene (5 g, 20.58 mmol), (R)-2-methylpiperazine (2.164 g, 21.61 mmol), sodium tert-butoxide (3.95 g, 41.15 mmol) and BINAP (0.512 g, 0.82 mmol) in anhydrous toluene (60 mL) was degassed under vacuum with inlet of nitrogen. TRIS(DIBENZYLIDENEACETONE)DIPALLADIUM(0) (0.377 g, 0.41 mmol) was added, the mixture again degassed. The resulting suspension was stirred at 100 °C for 6 hours under nitrogen. LCMS: Product formed. Cooled and evaporated. Residue diluted with diethyl ether (75 mL), filtered through Celite and the filtrates extracted with 2M HCl (2x30 mL). The combined aqueous layers were basified with solid NaOH to pH ~10, extracted with diethyl ether (2x50 mL), the organic extracts washed with water (2x10 mL) and brine, dried over mgSO4, filtered and evaporated to give crude product (3.2g, 59%) as an orange oil which was used without further purification.
出典と根拠
- ORDレコード
- ord-5ffc5c4a730b4c9fa67430c9657da268
- 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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