Diisopropylethylamine → HCID 67331064、化合物
反応式
[F:1][C:2]([F:8])([F:7])[CH2:3][C:4](O)=[O:5].CN(C(ON1N=NC2C=CC=NC1=2)=[N+](C)C)C.F[P-](F)(F)(F)(F)F.C(N(C(C)C)CC)(C)C.[C:42]1([C:48]2[O:49][C:50]3[CH:56]=[CH:55][C:54]([NH2:57])=[CH:53][C:51]=3[CH:52]=2)[CH:47]=[CH:46][CH:45]=[CH:44][CH:43]=1>ClCCl.C(OCC)(=O)C>[C:42]1([C:48]2[O:49][C:50]3[CH:56]=[CH:55][C:54]([NH:57][C:4](=[O:5])[CH2:3][C:2]([F:8])([F:7])[F:1])=[CH:53][C:51]=3[CH:52]=2)[CH:43]=[CH:44][CH:45]=[CH:46][CH:47]=1参加物
反応物 4
生成物 1
試薬・触媒・溶媒 2
実験手順
To 3,3,3-trifluoropropanoic acid (136 mg, 1.06 mmol) in dry dichloromethane (10 mL) was added HATU (468 mg, 1.23 mmol) and diisopropylethylamine (580 μL, 3.35 mmol). The mixture was then stirred at room temperature for 10 min. 2-phenylbenzofuran-5-amine (234 mg, 1.12 mmol) was then added and the resulting mixture was stirred at room temperature for 48 h. Ethyl acetate was added and the organic layer was washed once with saturated aqueous water. The combined organic layers were dried over anhydrous MgSO4 and evaporated. The resulting solid was purified by column chromatography eluting using a gradient (ethyl acetate/hexanes 1:3 v/v to ethyl acetate/hexanes 1:1 v/v) followed by trituration in ethyl acetate to afford 99.3 mg (28%) of the title compound (LCMS RT=6.62 min)
後処理
- stirringthe resulting mixture was stirred at room temperature for 48 h
- washthe organic layer was washed once with saturated aqueous water
- dry with materialThe combined organic layers were dried over anhydrous MgSO4
- customevaporated
- customThe resulting solid was purified by column chromatography
- washeluting
出典と根拠
- ORDレコード
- ord-07da71ba7d574f3cbd8def2a87ffe4a8
- 出典データセット
- uspto-grants-2013_08
- 特許番号
- US08518980B2
反応ノート
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