反応式
[I:1][C:2]1[CH:3]=[C:4]([CH:8]=[CH:9][C:10]=1[CH3:11])[C:5](Cl)=[O:6].C(N(CC)CC)C.[N:19]1([C:25]2[CH:26]=[C:27]([NH2:31])[CH:28]=[CH:29][CH:30]=2)[CH2:24][CH2:23][O:22][CH2:21][CH2:20]1>CN(C=O)C>[I:1][C:2]1[CH:3]=[C:4]([CH:8]=[CH:9][C:10]=1[CH3:11])[C:5]([NH:31][C:27]1[CH:28]=[CH:29][CH:30]=[C:25]([N:19]2[CH2:24][CH2:23][O:22][CH2:21][CH2:20]2)[CH:26]=1)=[O:6]参加物
5
反応条件
- 温度
- 80 °C
実験手順
3-Iodo-4-methylbenzoyl chloride (Intermediate 6) (19.5 g) was added portion-wise to a mixture of triethylamine (48 ml) and 3-(4-morpholinyl)benzenamine (Intermediate 8) (12.6 g) in DMF (150 ml) and the mixture was heated at 80° C. for 16 h. The solvent was removed under vacuum and the residue was dissolved in chloroform (200 ml). The organic layer was washed with water (2×100 ml), 2M sodium hydroxide solution (100 ml) and brine (100 ml), dried over magnesium sulphate, filtered and concentrated under vacuum The resulting yellow solid was triturated with diethyl ether and collected by filtration to yield the title compound as an off-white solid (20.0 g). The product was used in subsequent reactions without further purification.
後処理
- customThe solvent was removed under vacuum
- dissolutionthe residue was dissolved in chloroform (200 ml)
- washThe organic layer was washed with water (2×100 ml), 2M sodium hydroxide solution (100 ml) and brine (100 ml)
- dry with materialdried over magnesium sulphate
- filtrationfiltered
- concentrationconcentrated under vacuum The resulting yellow solid
- customwas triturated with diethyl ether
- filtrationcollected by filtration
出典と根拠
- ORDレコード
- ord-ef3be8a465a94d978fa7fdbe4ba68d92
- 出典データセット
- uspto-grants-2010_01
- 特許番号
- US07642276B2
関連ノート
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