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4-Iodophenol → 2-(4-Iodophenoxy)-4,6-dimethylpyrimidine

HRID 1752049
ノート
印刷プレビュー

反応式

HRID 1752049 の反応式
[I:1][C:2]1[CH:7]=[CH:6][C:5]([OH:8])=[CH:4][CH:3]=1.Cl[C:10]1[N:15]=[C:14]([CH3:16])[CH:13]=[C:12]([CH3:17])[N:11]=1.[H-].[Na+]>>[I:1][C:2]1[CH:7]=[CH:6][C:5]([O:8][C:10]2[N:15]=[C:14]([CH3:16])[CH:13]=[C:12]([CH3:17])[N:11]=2)=[CH:4][CH:3]=1
参加物実験手順出典と根拠反応ノート

参加物

4

反応物 3

HCID 108944-IodophenolHCID 205502-Chloro-4,6-dimethylpyrimidineHCID 24758Sodium hydride

生成物 1

HCID 577624972-(4-Iodophenoxy)-4,6-dimethylpyrimidine収率 68.4%

実験手順

Under an argon atmosphere, phosphorus oxychloride (2 ml) was added to 4,6-dimethyl-2-hydroxypyrimidine (400 mg), and the resulting mixture was stirred for 1 hour while heating the mixture to reflux. The reaction solution was cooled to room temperature, and the cooled solution was added in small portions to water. After adding sodium hydrogen carbonate in small portions to the resulting mixture to neutralize it, the mixture was extracted with ethyl acetate. Organic layer was washed twice with water and once with saturated brine, and dried over anhydrous sodium sulfate. After removing anhydrous sodium sulfate by filtration, the filtrate was concentrated to obtain 2-chloro-4,6-dimethylpyrimidine (350 mg). (2) In the same manner as in Reference Example 8, 4-iodophenol (223 mg) and 2-chloro-4,6-dimethylpyrimidine (157 mg) were reacted by using sodium hydride to obtain 2-(4-iodophenoxy)-4,6-dimethylpyrimidine (226 mg),

出典と根拠

ORDレコード
ord-9bf6712bb4484d41b662d9924ffbab77
出典データセット
uspto-grants-2015_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09162988B2

反応ノート

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