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Succinic anhydride → Succinic acid mono-(2,4,6-trimethylbenzyl) ester

HRID 507016
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HRID 507016 반응식
[CH3:1][C:2]1[CH:9]=[C:8]([CH3:10])[CH:7]=[C:6]([CH3:11])[C:3]=1[CH2:4][OH:5].[C:12]1(=[O:18])[O:17][C:15](=[O:16])[CH2:14][CH2:13]1.C(=O)([O-])[O-].[Cs+].[Cs+]>O1CCOCC1>[CH3:1][C:2]1[CH:9]=[C:8]([CH3:10])[CH:7]=[C:6]([CH3:11])[C:3]=1[CH2:4][O:5][C:12](=[O:18])[CH2:13][CH2:14][C:15]([OH:17])=[O:16]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 7922Succinic anhydrideHCID 10796Cesium carbonateHCID 201392,4,6-Trimethylbenzyl alcohol

생성물 1

HCID 68466934Succinic acid mono-(2,4,6-trimethylbenzyl) ester수율 46.62%

시약·촉매·용매 1

HCID 312751,4-Dioxane용매

실험 절차

A mixture of 1.50 g (0.01 mol) of 2,4,6-trimethylbenzyl alcohol, 1.00 g (0.01 mol) of succinic acid anhydride, 3.25 g (0.01 mol) of cesium carbonate, and 100 ml of dioxane was stirred at reflux temperature for 4 hours. The reaction mixture was cooled to room temperature and then filtered to remove the solid cesium carbonate. The solvent was removed under reduced pressure. The crude product was purified by column chromatography on silica gel (acetone-hexane) to provide 1.167 g of succinic acid mono-(2,4,6-trimethylbenzyl) ester (46.62%).

후처리

  1. temperatureat reflux temperature for 4 hours
  2. filtrationfiltered
  3. customto remove the solid cesium carbonate
  4. customThe solvent was removed under reduced pressure
  5. customThe crude product was purified by column chromatography on silica gel (acetone-hexane)

출처 및 근거

ORD 기록
ord-1fca4d2884b84a3f92b7a2dda51079a3
출처 데이터셋
uspto-grants-2010_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07786134B2

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