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Sodium hydride → HCID 69358200, 화합물

HRID 852637
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HRID 852637 반응식
[CH3:1][O:2][C:3](=[O:20])[C:4]1[CH:9]=[C:8]([O:10][CH2:11][CH3:12])[CH:7]=[C:6]([NH:13][C:14](=[O:19])[CH2:15][CH2:16][CH2:17]Cl)[CH:5]=1.[H-].[Na+]>C1COCC1.CCOC(C)=O>[CH3:1][O:2][C:3](=[O:20])[C:4]1[CH:5]=[C:6]([N:13]2[CH2:17][CH2:16][CH2:15][C:14]2=[O:19])[CH:7]=[C:8]([O:10][CH2:11][CH3:12])[CH:9]=1
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참가 물질

5

반응물 2

HCID 24758Sodium hydrideHCID 69356535HCID 69356535, 화합물

생성물 1

HCID 69358200HCID 69358200, 화합물수율 66.5%

시약·촉매·용매 2

HCID 8028Tetrahydrofuran용매HCID 8857Ethyl Acetate용매

실험 절차

3-(4-Chloro-butanoylamino)-5-ethoxy-benzoic acid methyl ester (D51) (7 g, 20 mmol, 1 equiv) in THF (50 ml) was treated portionwise with NaH (60% in mineral oil, 0.88 g, 22 mmol, 1.1 equiv) over 15 min at room temperature. The resulting mixture was stirred for 30 min and then diluted with AcOEt (300 ml). The resulting solution was washed with 2N aqueous HCl solution (200 ml), dried over MgSO4 and concentrated in vacuo. Recrystallisation of the residue from Et2O/hexane gave 3-ethoxy-5-(2-oxo-pyrrolidin-1-yl)-benzoic acid methyl ester (B11) (3.5 g, 66%) as white solid.

후처리

  1. washThe resulting solution was washed with 2N aqueous HCl solution (200 ml)
  2. dry with materialdried over MgSO4
  3. concentrationconcentrated in vacuo
  4. customRecrystallisation of the residue from Et2O/hexane

출처 및 근거

ORD 기록
ord-0ea6754d525041eb907d3c604d5027bb
출처 데이터셋
uspto-grants-2007_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07253198B2

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