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Ethyl Acetate → 2-{[(Benzyloxy)carbonyl]amino}-3-(3-{[(t-butoxycarbonyl)amino]methyl}-4-methoxyphenyl)-2-propenoic acid methyl ester
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Ethyl Acetate | HCID 8857 | — |
| 反応物 | 1,8-Diazabicyclo(5.4.0)undec-7-ene | HCID 81184 | — |
| 反応物 | Tert-butyl (5-formyl-2-methoxybenzyl)carbamate | HCID 22493931 | — |
| 反応物 | [(Benzyloxy)carbonyl]amino-2-(dimethoxyphosphoryl)acetate | HCID 131726531 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 2-{[(Benzyloxy)carbonyl]amino}-3-(3-{[(t-butoxycarbonyl)amino]methyl}-4-methoxyphenyl)-2-propenoic acid methyl ester | HCID 69485806 | — |
反応手順
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.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07244861B2 |
| 出典データセット | uspto-grants-2007_07 |
| ORD ID | ord-0477333a245b4dbf88326acc3540545d |
| 出典メモ | uspto-grants-2007_07 |