参与物
| 角色 | 名称 | HCID | 投料 |
|---|
| 反应物 | N,N’-1,2-乙烷基双[N-(羧甲基)-甘氨酸]三钠盐 | HCID 9008 | — |
| 反应物 | 重氮乙酸乙酯 | HCID 12192 | — |
| 反应物 | 梨醇酯 | HCID 14489 | — |
| 反应物 | trans-Body | HCID 24978618 | — |
| 催化剂 | Rhodium triphenyl acetate | HCID 71464060 | — |
| 溶剂 | 乙酸乙酯 | HCID 8857 | — |
| 产物 | Racemic ethyl cis-3-acetoxymethyl-2,2-dimethylcyclopropanecarboxylate | HCID 67120924 | — |
反应步骤
Rhodium triphenylacetate, 6.78 mg (0.01 mmol), was dissolved in 9.0 g of ethyl acetate, and 2.56 g (20.0 mmol) of 1-acetoxy-3-methyl-2-butene was added, then, the temperature thereof was raised to 50° C. Into this solution, a solution composed of 1.14 g (10.0 mmol) of ethyl diazoacetate and 3.6 g of ethyl acetate was dropped over a period of 2 hours, and the mixture was, thermally kept at the same temperature for 0.5 hours. To this solution was added an aqueous solution containing 0.5 mol of trisodium ethylenediaminetetraacetate per liter and the solution was mixed and separated, and a solution containing 1.82 g of ethyl 3-acetoxymethyl-2,2-dimethylcyclopropanecarboxylate was obtained (yield based on ethyl diazoacetate: 84.8%). The cis body/trans body ratio was 72/28.
来源与证据
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 专利号 | US07928253B2 |
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| 来源数据集 | uspto-grants-2011_04 |
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| ORD ID | ord-d0790c9840c94fa5bdb44412e7d5bb07 |
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| 来源说明 | uspto-grants-2011_04 |
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