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Sodium hydride → HCID 131717242、化合物

HRID 466681
ノート
印刷プレビュー

反応式

HRID 466681 の反応式
[H-].[Na+].[Cl:3][C:4]1[N:12]=[CH:11][N:10]=[C:9]2[C:5]=1[NH:6][C:7]([CH2:13][CH2:14][CH3:15])=[N:8]2.[C:16]([O:20][C:21]([C:23]1[C:24]([C:29]2[CH:34]=[CH:33][C:32]([CH2:35]Br)=[CH:31][CH:30]=2)=[CH:25][CH:26]=[CH:27][CH:28]=1)=[O:22])([CH3:19])([CH3:18])[CH3:17]>CN(C=O)C>[Cl:3][C:4]1[N:12]=[CH:11][N:10]=[C:9]2[C:5]=1[N:6]=[C:7]([CH2:13][CH2:14][CH3:15])[N:8]2[CH2:35][C:32]1[CH:33]=[CH:34][C:29]([C:24]2[CH:25]=[CH:26][CH:27]=[CH:28][C:23]=2[C:21]([O:20][C:16]([CH3:19])([CH3:18])[CH3:17])=[O:22])=[CH:30][CH:31]=1
参加物反応条件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 24758Sodium hydrideHCID 9906257tert-Butyl 4'-(bromomethyl)biphenyl-2-carboxylateHCID 190122236-Chloro-8-propylpurine

生成物 1

HCID 131717242HCID 131717242、化合物

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

反応条件

温度
40 °C

実験手順

To a suspension of NaH (0.20 g) in dry DMF (3 ml), 6-chloro-8-propyl-purine (0.06 g, 0.3 mmol) was added, and the mixture was stirred at 40° C. for 20 minutes. t-Butyl-4-bromomethylbiphenyl-2'-carboxylate (0.11 g, 0.31 mmol) was then added at room temperature and stirring continued for 3 hours at 40° C. The content of the flask was poured into ice-water (100 ml and extracted with ethylacetate. The organic phase was separated and dried over MgSO4. Removal of the solvent under reduced pressure gave the crude product which was then purified by flash-chromatography on silica-gel using ethylacetate-hexane (1:1). The pure titled compound was obtained as a glass-like solid (0.073 g, 53%).

後処理

  1. additionwas added
  2. stirringstirring
  3. waitcontinued for 3 hours at 40° C
  4. extractionextracted with ethylacetate
  5. customThe organic phase was separated
  6. dry with materialdried over MgSO4
  7. customRemoval of the solvent under reduced pressure
  8. customgave the crude product which
  9. customwas then purified by flash-chromatography on silica-gel

出典と根拠

ORDレコード
ord-9d707d9f9d664bd288e46dc122b8f8aa
出典データセット
uspto-grants-1992_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05157026

反応ノート

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