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Sodium Thiosulfate → HCID 22063528, 화합물

HRID 1828464
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HRID 1828464 반응식
[OH:1][CH2:2][CH:3]1[CH2:5][CH:4]1[C:6]1[C:11](=[O:12])[N:10]2[CH:13]=[CH:14][C:15]([CH2:17][CH2:18][C:19]3[S:20][CH:21]=[C:22]([CH:24]([CH3:26])[CH3:25])[N:23]=3)=[CH:16][C:9]2=[N:8][C:7]=1[N:27]1[CH2:32][CH2:31][O:30][CH2:29][CH2:28]1.CC(C)=[O:35].OS(O)(=O)=O.O=[Cr](=O)=O.S([O-])([O-])(=O)=S.[Na+].[Na+]>CC(C)=O>[CH:24]([C:22]1[N:23]=[C:19]([CH2:18][CH2:17][C:15]2[CH:14]=[CH:13][N:10]3[C:11](=[O:12])[C:6]([CH:4]4[CH2:5][CH:3]4[C:2]([OH:35])=[O:1])=[C:7]([N:27]4[CH2:32][CH2:31][O:30][CH2:29][CH2:28]4)[N:8]=[C:9]3[CH:16]=2)[S:20][CH:21]=1)([CH3:26])[CH3:25]
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참가 물질

5

반응물 3

HCID 24477Sodium ThiosulfateHCID 22063735HCID 22063735, 화합물HCID 131709961Jones' reagent2회

생성물 1

HCID 22063528HCID 22063528, 화합물수율 4%

시약·촉매·용매 1

HCID 180Acetone용매

실험 절차

3-[2-(Hydroxymethyl)cyclopropyl]-8-[2-(4-isopropyl-1,3-thiazol-2-yl)ethyl]-2-morpholino-4H-pyrido[1,2-a]pyrimidin-4-one (55 mg, 0.121 mmol) dissolved in acetone (10 ml) was added dropwise with Jones' reagent (130 μl, 0.363 mmol) under ice cooling with and stirred for 2 hours. Then, the reaction solution was further added with Jones' reagent (165 μl) and stirred for 2 hours. Then, the reaction was stopped with saturated sodium thiosulfate, and the reaction solution was extracted with chloroform. The organic layer was dried over magnesium sulfate and concentrated under reduced pressure. The resulting residue was purified by thin layer silica gel chromatography (chloroform:methanol=10:1) to obtain 2.2 mg (4%) of the title compound as yellow crystals.

후처리

  1. stirringstirred for 2 hours
  2. extractionthe reaction solution was extracted with chloroform
  3. dry with materialThe organic layer was dried over magnesium sulfate
  4. concentrationconcentrated under reduced pressure
  5. customThe resulting residue was purified by thin layer silica gel chromatography (chloroform:methanol=10:1)

출처 및 근거

ORD 기록
ord-20a0cc9e0faa400983fe2757a788a920
출처 데이터셋
uspto-grants-2006_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07056917B2

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