Hydrogen Peroxide → 3-[4-(3-Cyclopentyloxy-4-methoxyphenyl)-2-oxo-pyrrolidin-1-yl]benzamide

HRID 1727159

반응식

HRID 1727159 반응식
[CH:1]1([O:6][C:7]2[CH:8]=[C:9]([CH:15]3[CH2:19][N:18]([C:20]4[CH:21]=[C:22]([CH:25]=[CH:26][CH:27]=4)[C:23]#[N:24])[C:17](=[O:28])[CH2:16]3)[CH:10]=[CH:11][C:12]=2[O:13][CH3:14])[CH2:5][CH2:4][CH2:3][CH2:2]1.[OH-].[Na+].OO.[OH:33]S(O)(=O)=O>C(O)C>[CH:1]1([O:6][C:7]2[CH:8]=[C:9]([CH:15]3[CH2:19][N:18]([C:20]4[CH:21]=[C:22]([CH:25]=[CH:26][CH:27]=4)[C:23]([NH2:24])=[O:33])[C:17](=[O:28])[CH2:16]3)[CH:10]=[CH:11][C:12]=2[O:13][CH3:14])[CH2:2][CH2:3][CH2:4][CH2:5]1

참가 물질

6

반응물 4

HCID 784Hydrogen PeroxideHCID 1118Sulfuric AcidHCID 14798Sodium HydroxideHCID 104746693-[4-(3-Cyclopentyloxy-4-methoxy-phenyl)-2-oxo-pyrrolidin-1-yl]benzonitrile

생성물 1

HCID 99525243-[4-(3-Cyclopentyloxy-4-methoxyphenyl)-2-oxo-pyrrolidin-1-yl]benzamide수율 94%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

To 12.5 mg of benzonitrile 42 (0.033 mmol) in 0.5 mL of ethanol was added 2 μL of a 25% NaOH solution followed by 29 μL of 35% H2O2. The temperature of the reaction mixture was kept at 50° C. for 3 h. Upon completion, 5% H2SO4 was added until the mixture was neutral (pH 7). The reaction mixture was extracted with EtOAc and dried with MgSO4. Concentration and purification of the residue by column chromatography on silica gel gave the desired product as a white solid. Yield: 94%.

후처리

  1. extractionThe reaction mixture was extracted with EtOAc
  2. dry with materialdried with MgSO4
  3. concentrationConcentration and purification of the residue by column chromatography on silica gel

출처 및 근거

ORD 기록
ord-44a298f8c48148c9afa965841923487c
출처 데이터셋
uspto-grants-2009_02
특허 번호
US07495016B2

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