反応式
[CH:1]([C:3]1[CH:4]=[CH:5][C:6]([O:18][CH3:19])=[C:7]([CH:17]=1)[CH2:8][NH:9][C:10](=[O:16])[O:11][C:12]([CH3:15])([CH3:14])[CH3:13])=O.[CH2:20]([O:27][C:28]([NH:30][CH:31](P(OC)(OC)=O)[C:32]([O-:34])=[O:33])=[O:29])[C:21]1[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=1.[CH2:41]1CCN2C(=NCCC2)CC1.C(OCC)(=O)C>ClCCl>[CH3:41][O:34][C:32](=[O:33])[C:31]([NH:30][C:28]([O:27][CH2:20][C:21]1[CH:22]=[CH:23][CH:24]=[CH:25][CH:26]=1)=[O:29])=[CH:1][C:3]1[CH:4]=[CH:5][C:6]([O:18][CH3:19])=[C:7]([CH2:8][NH:9][C:10]([O:11][C:12]([CH3:15])([CH3:14])[CH3:13])=[O:16])[CH:17]=1参加物
6
反応物 4
生成物 1
試薬・触媒・溶媒 1
実験手順
2.65 g of t-butyl N-(5-formyl-2-methoxybenzyl)carbamate, 3.81 g of methyl 2-([(benzyloxy)carbonyl]amino-2-(dimethoxyphosphoryl)acetate and 1.75 g of 1,8-diazabicyclo[5,4,0]-7-undecene were dissolved in 50 ml of dichloromethane, followed by stirring for 15 hours at room temperature. 300 ml of ethyl acetate was added, and the organic layer was successively washed with 150 ml of water and 150 ml of brine, dried over magnesium sulfate and concentrated. The residue was purified by silica gel column chromatography, and 4.09 g of 2-{[(benzyloxy)carbonyl]amino}-3-(3-{[(t-butoxycarbonyl)amino]methyl}-4-methoxyphenyl)-2-propenoic acid methyl ester was obtained as a colorless solid.
後処理
- washthe organic layer was successively washed with 150 ml of water and 150 ml of brine
- dry with materialdried over magnesium sulfate
- concentrationconcentrated
- customThe residue was purified by silica gel column chromatography
出典と根拠
- ORDレコード
- ord-0477333a245b4dbf88326acc3540545d
- 出典データセット
- uspto-grants-2007_07
- 特許番号
- US07244861B2
関連ノート
読み込み中…