参与物
| 角色 | 名称 | HCID | 投料 |
|---|
| 反应物 | 4-苄氧基-3-甲氧基苯甲醛 | HCID 75506 | — |
| 反应物 | 叠氮乙酸甲酯 | HCID 4020482 | — |
| 反应物 | 钠 | HCID 5360545 | — |
| 反应物 | 甲醇钠 | HCID 10942334 | — |
| 溶剂 | (5BETA,17BETA)-17-羟基-17-(甲基-D3)-2'H-雄甾-2-烯并[3,2-C]吡唑-5'(1'H)-酮 | HCID 887 | — |
| 产物 | Methyl-2-azido-3-[4'-(benzyloxy)-3'-methoxyphenyl]prop-2-enoate | HCID 72390540 | 73% |
反应步骤
A solution of the 4-Benzyloxy-3-methoxy-benzaldehyde (12.0 g, 49.6 mmol) and methyl azidoacetate (23 g, 0.200 mol) in methanol (50 mL) was added over 30 min to a cooled (ice-salt bath) solution of sodium methoxide which had been prepared from addition of methanol (80 mL) to sodium (3.4 g, 0.149 mol). The reaction mixture was stirred at 0° C. for 45 min, during this time a thick cream precipitate formed, and then stood in the freezer overnight. Ice-cold water was added and the precipitate was removed by filtration and dried to give methyl-2-azido-3-[4′-(benzyloxy)-3′-methoxyphenyl]prop-2-enoate (55) (12.2 g, 73%) which was used in the next step without purification.
来源与证据
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 专利号 | US07094798B1 |
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| 来源数据集 | uspto-grants-2006_08 |
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| ORD ID | ord-d9e8ac3d46b14af1810494a565aed42a |
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| 来源说明 | uspto-grants-2006_08 |
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