Acetic acid, 2-(triphenylphosphoranylidene)-, methyl ester → 4-Tert-butyl 1-methyl 2-(triphenylphosphoranylidene)succinate

HRID 70874

반응식

HRID 70874 반응식
[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]

참가 물질

4

반응물 2

HCID 17453Acetic acid, 2-(triphenylphosphoranylidene)-, methyl esterHCID 79177tert-Butyl bromoacetate

생성물 1

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

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

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).

후처리

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

출처 및 근거

ORD 기록
ord-d53be708fee74f9097fc77a08a72f3d1
출처 데이터셋
uspto-grants-2014_09
특허 번호
US08822534B2

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