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m-Chloroperbenzoic acid → 2-Isopropyl-7-(2-methanesulfinyl-ethoxy)-4-(5-methyl-1H-pyrazol-3-ylamino)-2H-phthalazin-1-one

HRID 1783713
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HRID 1783713 반응식
[CH:1]([N:4]1[N:13]=[C:12]([NH:14][C:15]2[CH:19]=[C:18]([CH3:20])[NH:17][N:16]=2)[C:11]2[C:6](=[CH:7][C:8]([O:21][CH2:22][CH2:23][S:24][CH3:25])=[CH:9][CH:10]=2)[C:5]1=[O:26])([CH3:3])[CH3:2].ClC1C=C(C=CC=1)C(OO)=[O:32]>C(Cl)Cl>[CH:1]([N:4]1[N:13]=[C:12]([NH:14][C:15]2[CH:19]=[C:18]([CH3:20])[NH:17][N:16]=2)[C:11]2[C:6](=[CH:7][C:8]([O:21][CH2:22][CH2:23][S:24]([CH3:25])=[O:32])=[CH:9][CH:10]=2)[C:5]1=[O:26])([CH3:2])[CH3:3]
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참가 물질

4

반응물 2

HCID 70297m-Chloroperbenzoic acidHCID 247534922-Isopropyl-4-(5-methyl-1H-pyrazol-3-ylamino)-7-(2-methylsulfanyl-ethoxy)-2H-phthalazin-1-one

생성물 1

HCID 247535912-Isopropyl-7-(2-methanesulfinyl-ethoxy)-4-(5-methyl-1H-pyrazol-3-ylamino)-2H-phthalazin-1-one수율 16.7%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

To a solution of 2-isopropyl-4-(5-methyl-1H-pyrazol-3-ylamino)-7-(2-methylsulfanyl-ethoxy)-2H-phthalazin-1-one (0.077 g, 0.23 mmol) in DCM (2 ml), was added m-chloro-peroxybenzoic acid (0.040 g, 0.23 mmol) portion wise. The solution was stirred at RT for 1 hour. After this time LC-MS indicated complete consumption of starting material and the solvent was removed under vacuum. Preparative thin layer chromatography (elution: 50% EtOAc, 50% EtOH) afforded the title compound (0.015 g, 14% yield) as a pale yellow solid.

후처리

  1. customconsumption of starting material
  2. customthe solvent was removed under vacuum
  3. washPreparative thin layer chromatography (elution: 50% EtOAc, 50% EtOH)

출처 및 근거

ORD 기록
ord-ced49b7e30a54950abb6c681fcae2c93
출처 데이터셋
uspto-grants-2009_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07501410B2

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