Water → 6-(3,4-Dimethoxyphenyl)-2-methyl-4-(2,4,6-trimethylphenoxy)pyrimidine

HRID 4341

反応式

HRID 4341 の反応式
[CH3:1][C:2]1[CH:7]=[C:6]([CH3:8])[CH:5]=[C:4]([CH3:9])[C:3]=1[OH:10].[H-].[Na+].Cl[C:14]1[CH:19]=[C:18]([C:20]2[CH:25]=[CH:24][C:23]([O:26][CH3:27])=[C:22]([O:28][CH3:29])[CH:21]=2)[N:17]=[C:16]([CH3:30])[N:15]=1.O>CN(C)C=O>[CH3:29][O:28][C:22]1[CH:21]=[C:20]([C:18]2[N:17]=[C:16]([CH3:30])[N:15]=[C:14]([O:10][C:3]3[C:4]([CH3:9])=[CH:5][C:6]([CH3:8])=[CH:7][C:2]=3[CH3:1])[CH:19]=2)[CH:25]=[CH:24][C:23]=1[O:26][CH3:27]

参加物

6

反応物 4

HCID 962WaterHCID 106982,4,6-TrimethylphenolHCID 24758Sodium hydrideHCID 201522714-Chloro-6-(3,4-dimethoxyphenyl)-2-methylpyrimidine

生成物 1

HCID 201522566-(3,4-Dimethoxyphenyl)-2-methyl-4-(2,4,6-trimethylphenoxy)pyrimidine収率 71.2%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

To a solution of 2,4,6-trimethylphenol (1.03 g) in N,N-dimethylformamide (20 ml) was added sodium hydride (60% in oil, 0.30 g), and stirred at ambient temperature for 5 minutes. To the solution was added 4-chloro-6-(3,4-dimethoxyphenyl)-2-methylpyrimidine (2.0 g), and the mixture was stirred at ambient temperature for 18 hours. The solution was poured into water (300 ml), and extracted with ethyl acetate. The organic layer was washed with brine, dried over sodium sulfate and evaporated. The residue was chromatographed on silica gel eluting with chloroform to give 6-(3,4-dimethoxyphenyl)-2-methyl-4-(2,4,6-trimethylphenoxy)pyrimidine (1.96 g).

後処理

  1. stirringthe mixture was stirred at ambient temperature for 18 hours
  2. extractionextracted with ethyl acetate
  3. washThe organic layer was washed with brine
  4. dry with materialdried over sodium sulfate
  5. customevaporated
  6. customThe residue was chromatographed on silica gel eluting with chloroform

出典と根拠

ORDレコード
ord-8c0e664d28f44521b67fd86394cabfa0
出典データセット
uspto-grants-1988_02
特許番号
US04725600

関連ノート

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