参与物
| 角色 | 名称 | HCID | 投料 |
|---|
| 反应物 | 氢化钠 | HCID 24758 | — |
| 反应物 | 溴甲基环丙烷 | HCID 81503 | — |
| 反应物 | 碳酸氢钠 | HCID 516892 | — |
| 反应物 | 2-(Diethoxyphosphoryl)acetic acid para-methoxybenzyl ester | HCID 54020927 | — |
| 溶剂 | 乙醚 | HCID 3283 | — |
| 溶剂 | N,N-二甲基甲酰胺 | HCID 6228 | — |
| 产物 | 2-(Diethoxyphosphoryl)-3-cyclopropylproprionic acid 4-methoxybenzyl ester | HCID 54084105 | 60.9% |
反应步骤
To a suspension of 60% sodium hydride in mineral oil (0.840 g, 21.0 mmol) in DMF (100 mL) was added a solution of 2-(diethoxyphosphoryl)acetic acid 4-methoxybenzyl ester (6.04 g, 19.1 mmol) from Step A in DMF (10 mL). The reaction mixture was stirred for 30 min at room temperature. Bromomethylcyclopropane (2.4 mL, 24.8 mmol) was added and the reaction mixture was stirred at room temperature for 12 h. The reaction mixture was diluted with diethyl ether, poured into saturated sodium bicarbonate, and extracted three times with diethyl ether. The organic layers were combined, washed with saturated sodium chloride, dried over sodium sulfate, and filtered. The volatiles were removed in vacuo and the residue was purified by FC (40% ethyl acetate in hexanes) to afford 4.31 g of the title compound.
来源与证据
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 专利号 | US07091211B2 |
|---|
| 来源数据集 | uspto-grants-2006_08 |
|---|
| ORD ID | ord-e31142420d854a6b93bb0fdda233b4cb |
|---|
| 来源说明 | uspto-grants-2006_08 |
|---|