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Sodium Thiosulfate → HCID 22063528、化合物

HRID 1828464
ノート
印刷プレビュー

反応式

HRID 1828464 の反応式
[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]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 24477Sodium ThiosulfateHCID 22063735HCID 22063735、化合物HCID 131709961Jones' reagent2 回

生成物 1

HCID 22063528HCID 22063528、化合物収率 4%

試薬・触媒・溶媒 1

HCID 180Acetone溶媒

実験手順

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.

後処理

  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)

出典と根拠

ORDレコード
ord-20a0cc9e0faa400983fe2757a788a920
出典データセット
uspto-grants-2006_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07056917B2

反応ノート

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