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

HRID 4341

반응식

HRID 4341 반응식
[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]

참가 물질

6

반응물 4

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

생성물 1

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

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-8c0e664d28f44521b67fd86394cabfa0
출처 데이터셋
uspto-grants-1988_02
특허 번호
US04725600

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