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Sodium Hydroxide → HCID 69357330, 화합물

HRID 852544
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HRID 852544 반응식
[CH3:1][O:2][C:3](=[O:17])[C:4]1[CH:13]=[C:12]([O:14][CH2:15][CH3:16])[CH:11]=[C:6]([C:7]([O:9]C)=[O:8])[CH:5]=1.[OH-].[Na+]>CO>[CH3:1][O:2][C:3](=[O:17])[C:4]1[CH:13]=[C:12]([O:14][CH2:15][CH3:16])[CH:11]=[C:6]([C:7]([OH:9])=[O:8])[CH:5]=1
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참가 물질

4

반응물 2

HCID 14798Sodium HydroxideHCID 68538880HCID 68538880, 화합물

생성물 1

HCID 69357330HCID 69357330, 화합물수율 82.1%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

To a solution of 5-ethoxy-isophthalic acid dimethyl ester (D43) (22 g, 92.4 mmol, 1 equiv) in MeOH (440 ml) was added 1N aqueous NaOH solution (87.8 ml, 87.8 mmol, 0.95 equiv) and the resulting solution was stirred at room temperature for 17 h. Most of the MeOH was removed in vacuo and the residue was partitioned between AcOEt and 1N aqueous NaOH solution. The aqueous layer was extracted with AcOEt, acidified to pH 1 and re-extracted with AcOEt. The second organic extract was dried over MgSO4 and concentrated in vacuo to give 5-ethoxy-isophthalic acid monomethyl ester (D45) (17 g, 82%) as a white solid. [M+H+ NH3]+=242.0, RT=2.79 min

후처리

  1. customMost of the MeOH was removed in vacuo
  2. customthe residue was partitioned between AcOEt and 1N aqueous NaOH solution
  3. extractionThe aqueous layer was extracted with AcOEt
  4. extractionre-extracted with AcOEt
  5. extractionThe second organic extract
  6. dry with materialwas dried over MgSO4
  7. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-78fa2a39409a4fab9a8b2293e0d49f36
출처 데이터셋
uspto-grants-2007_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07253198B2

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