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Sodium hydride → HCID 68777402, 화합물

HRID 2061576
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HRID 2061576 반응식
[CH3:1][O:2][C:3]([C:5]1([NH:18][C:19](=[O:24])[CH2:20][CH2:21][CH2:22]Cl)[CH2:10][CH2:9][N:8]([C:11]([O:13][C:14]([CH3:17])([CH3:16])[CH3:15])=[O:12])[CH2:7][CH2:6]1)=[O:4].[H-].[Na+]>C1COCC1>[CH3:1][O:2][C:3]([C:5]1([N:18]2[CH2:22][CH2:21][CH2:20][C:19]2=[O:24])[CH2:10][CH2:9][N:8]([C:11]([O:13][C:14]([CH3:17])([CH3:16])[CH3:15])=[O:12])[CH2:7][CH2:6]1)=[O:4]
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참가 물질

4

반응물 2

HCID 24758Sodium hydrideHCID 68779529HCID 68779529, 화합물

생성물 1

HCID 68777402HCID 68777402, 화합물수율 58%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

실험 절차

The ester compound in dry THF (15 mL) was added to a suspension of NaH (352 mgs, 8.81 mmol) in dry THF (3 mL) and stirred at room temperature for 16 hours. The reaction mixture was then quenched with water (4 mL), diluted with ethyl acetate (60 mL), dried over MgSO4, filtered, and purified by flash chromatography on silica gel with stepwise elution using 50% ethyl acetate/hexanes to 100% ethyl acetate/hexanes gave 4-(2-oxo-pyrrolidin-1-yl)-piperidine-1,4-dicarboxylic acid 1-tert-butyl ester 4-methyl ester (1.28 g, 58.0% yield).

후처리

  1. customThe reaction mixture was then quenched with water (4 mL)
  2. additiondiluted with ethyl acetate (60 mL)
  3. dry with materialdried over MgSO4
  4. filtrationfiltered
  5. custompurified by flash chromatography on silica gel with stepwise elution

출처 및 근거

ORD 기록
ord-c643e9e54fac44a0aeac1d55f6b734aa
출처 데이터셋
uspto-grants-2012_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08283357B2

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