反応式
[CH2:1]([O:3][C:4](=[O:15])[C:5]1[CH:10]=[CH:9][C:8]([C:11](=[O:14])[CH2:12]Br)=[CH:7][CH:6]=1)[CH3:2].[CH3:16][C:17]1[NH:21][C:20](=[O:22])[C:19]([C:29]2[CH:34]=[CH:33][CH:32]=[CH:31][CH:30]=2)([C:23]2[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=2)[N:18]=1.C(=O)([O-])[O-].[K+].[K+].C1CCCCC1.C(OCC)(=O)C>CC(C)=O.C(OCC)(=O)C>[CH2:1]([O:3][C:4](=[O:15])[C:5]1[CH:10]=[CH:9][C:8]([C:11](=[O:14])[CH2:12][N:21]2[C:20](=[O:22])[C:19]([C:29]3[CH:30]=[CH:31][CH:32]=[CH:33][CH:34]=3)([C:23]3[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=3)[N:18]=[C:17]2[CH3:16])=[CH:7][CH:6]=1)[CH3:2]参加物
反応物 4
生成物 1
試薬・触媒・溶媒 2
反応条件
- 温度
- 70 °C
実験手順
To a mixture of 4-(2-bromo-acetyl)-benzoic acid ethyl ester (812 mg, 3 mmol) and 2-methyl-5,5-diphenyl-3,5-dihydro-imidazol-4-one (750 mg, 3 mmol) in 12 mL acetone, potassium carbonate (502 mg, 3.6 mmol) is added and the reaction mixture is heated at 70° C. for 5 min in the microwave oven (Biotage Initiator). The mixture is cooled to room temperature, filtered and the filtrate evaporated to yield the crude product which is subjected to flash chromatography. ISCO Companion CombiFlash, 80 g silica gel, cyclohexane/ethyl acetate, gradient, ethyl acetate 0-100% to yield 4-[2-(2-methyl-5-oxo-4,4-diphenyl4,5-dihydro-imidazol-1-yl)-acetyl]-benzoic acid ethyl ester (635 mg, 45%) as light yellow solid. LC/MS at 254 nm; [M+H] 441; Rt 3.613 min.
後処理
- additionis added
- temperatureThe mixture is cooled to room temperature
- filtrationfiltered
- customthe filtrate evaporated
- customto yield the crude product which
出典と根拠
- ORDレコード
- ord-f9d8a6508a3d42dbae724ee41ebb2115
- 出典データセット
- uspto-grants-2010_08
- 特許番号
- US07786155B2
関連ノート
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