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Dimethylformamide → HCID 57927312、化合物

HRID 889166
ノート
印刷プレビュー

反応式

HRID 889166 の反応式
[N:1]1[NH:2][C:3](=[O:10])[N:4]2[CH:9]=[CH:8][CH:7]=[N:6][C:5]=12.[Br:11][CH2:12][CH2:13][CH2:14]Br.[H-].[Na+].CN(C)C=O>C(OCC)(=O)C.O>[Br:11][CH2:12][CH2:13][CH2:14][N:2]1[C:3](=[O:10])[N:4]2[CH:9]=[CH:8][CH:7]=[N:6][C:5]2=[N:1]1
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 6228DimethylformamideHCID 80011,3-Dibromopropane2 回HCID 24758Sodium hydride2 回HCID 20551098[1,2,4]Triazolo[4,3-a]pyrimidin-3(2H)-one

生成物 1

HCID 57927312HCID 57927312、化合物

試薬・触媒・溶媒 2

HCID 962Water溶媒
HCID 8857
Ethyl Acetate
溶媒

実験手順

A mixture of 2H-[1,2,4]triazolo[4,3-a]pyrimidin-3-one (CAS 63206-77-9) (1.0 g), 1,3-dibromopropane (1.55 ml), sodium hydride (60% in oil) (353 mg) and N,N-dimethylformamide (20 ml) was stirred at room temperature for one day. After further addition of 1,3-dibromopropane (3.88 ml) and sodium hydride (60% in oil) (353 mg), stirring was continued at 80° C. for 2 hours. Water was added to the reaction mixture, and extraction was performed with ethyl acetate. The organic layer was washed with brine and dried over anhydrous magnesium sulfate. After filtration, the solvent was distilled off under reduced pressure. The residue was purified by silica gel column chromatography to obtain the title compound (190 mg).

後処理

  1. stirringstirring
  2. waitwas continued at 80° C. for 2 hours
  3. washThe organic layer was washed with brine
  4. dry with materialdried over anhydrous magnesium sulfate
  5. filtrationAfter filtration
  6. distillationthe solvent was distilled off under reduced pressure
  7. customThe residue was purified by silica gel column chromatography

出典と根拠

ORDレコード
ord-cfd4c2862fc64629ab7022e8bd10b725
出典データセット
uspto-grants-2012_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08252810B2

反応ノート

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このページの内容参加物実験手順後処理出典と根拠反応ノート