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HRID 399348生成日期:2026年10月23日

(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 → 甲基丁二酸二甲酯

https://huagongshe.com/zh-CN/reaction/399348

反应方程式

参与物

角色名称HCID投料
反应物(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—
反应物衣康酸二甲酯HCID 69240—
反应物HCID 178418361HCID 178418361—
催化剂1,1'-Bis[2,4,8,10-tetrakis(tert-butyl)-dibenzo[d,f][1,3,2]dioxaphosphepin-6-yl]ferroceneHCID 131720875—
溶剂MeOH tetrahydrofuranHCID 21899815—
产物甲基丁二酸二甲酯HCID 1535099.1%

反应步骤

A mixture of 33 mg (0.031 mmol) of the ferrocenyl bis(phosphonite) prepared in Example 1 and 12 mg (0.031 mmol) of bis(bicyclo[2.2.1]hepta-2,5-diene)rhodium(I) perchlorate in 2 mL of methanol/tetrahydrofuran (1:1) solution is stirred for two hours. Then, to the resultant solution of rhodium complex is added a solution of 490 mg (3.1 mmol) of dimethyl itaconate and 13 mL of methanol in a pressure reactor. The reactor is then pressurized to 1018 psi with hydrogen and the reaction is stirred at ambient temperature for 88 hours. 1H nmr analysis of the reaction mixtures shows a 100% conversion of dimethyl itaconate starting material to product. Workup of the reaction mixture gives 492 mg (99% yield) of desired dimethyl 2-methylsuccinate.

来源与证据

DOI10.6084/m9.figshare.5104873.v1
专利号US05817850
来源数据集uspto-grants-1998_10
ORD IDord-01ee56ea5f4542ab891ac9b67fc5cba5
来源说明uspto-grants-1998_10