反応式
COc1cc(I)ccc1Br.NC1COC1>CC(C)(C)[O-].CC1(C)c2cccc(P(c3ccccc3)c3ccccc3)c2Oc2c(P(c3ccccc3)c3ccccc3)cccc21.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]>COc1cc(NC2COC2)ccc1Br参加物
反応物 2
生成物 1
試薬・触媒・溶媒 4
反応条件
- 温度
- 80 °C
実験手順
A solution of 1-bromo-4-iodo-2-methoxybenzene (0.60 g, 1.92 mmol) dissolved in toluene (15 mL) was treated with oxetan-3-amine (0.140 g, 1.92 mmol), SODIUM TERT-BUTOXIDE (0.221 g, 2.30 mmol), XANTPHOS (0.111 g, 0.19 mmol) and TRIS(DIBENZYLIDENEACETONE)DIPALLADIUM(0) (0.044 g, 0.05 mmol) under nitrogen. The resulting mixture was stirred at 80 °C in a sealed tube for 2 hours. The reaction mixture was diluted with water (10 mL), and extracted with ethyl acetate (3x 20 mL). The organic was dried over MgSO4, filtered and evaporated to afford crude product. The crude product was purified by flash silica chromatography, elution 0-30% EtOAc in Heptane. Pure fractions were evaporated to dryness to afford N-(4-bromo-3-methoxyphenyl)oxetan-3-amine (0.177 g, 35.8 %) as a beige solid.
出典と根拠
- ORDレコード
- ord-29003fa36fea4ddebef83b29dba29c7c
- 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
読み込み中…