甲氧甲酰基亚甲基三苯基膦 → 4-Tert-butyl 1-methyl 2-(triphenylphosphoranylidene)succinate

HRID 70874

反应方程式

HRID 70874 反应方程式
[CH3:1][O:2][C:3](=[O:24])[CH:4]=[P:5]([C:18]1[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=1)([C:12]1[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=1)[C:6]1[CH:11]=[CH:10][CH:9]=[CH:8][CH:7]=1.Br[CH2:26][C:27]([O:29][C:30]([CH3:33])([CH3:32])[CH3:31])=[O:28]>C(Cl)Cl>[CH3:1][O:2][C:3](=[O:24])[C:4](=[P:5]([C:6]1[CH:11]=[CH:10][CH:9]=[CH:8][CH:7]=1)([C:18]1[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=1)[C:12]1[CH:13]=[CH:14][CH:15]=[CH:16][CH:17]=1)[CH2:26][C:27]([O:29][C:30]([CH3:33])([CH3:32])[CH3:31])=[O:28]

参与物

4

反应物 2

HCID 17453甲氧甲酰基亚甲基三苯基膦HCID 79177溴乙酸叔丁酯

产物 1

HCID 110157884-Tert-butyl 1-methyl 2-(triphenylphosphoranylidene)succinate

试剂、催化剂与溶剂 1

HCID 6344二氯甲烷溶剂

实验过程

To a solution of (triphenylphosphanylidene)-acetic acid methyl ester (2.26 g, 6.77 mmol) in methylene chloride (25 mL) is added t-butyl bromoacetate (1.32 g, 6.77 mmol) and the mixture is stirred at room temperature for 48 hours. The solvent is removed under reduced pressure and the residue is purified by column chromatography using a gradient of 80-100% heptane/EtOAc to afford 2-(triphenylphosphanylidene)-succinic acid 4-tert-butyl ester 1-methyl ester. MS 449.3 (M+1).

后处理

  1. customThe solvent is removed under reduced pressure
  2. customthe residue is purified by column chromatography

来源与证据

ORD记录
ord-d53be708fee74f9097fc77a08a72f3d1
来源数据集
uspto-grants-2014_09
专利号
US08822534B2

关联笔记

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