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Potassium Carbonate → 3-(2-methoxyethoxy)-1-methyl-4-(4-methylphenyl)-1H-pyrazol-5-ylamine

HRID 397280
ノート
印刷プレビュー

反応式

HRID 397280 の反応式
[NH2:1][C:2]1[N:6]([CH3:7])[N:5]=[C:4]([OH:8])[C:3]=1[C:9]1[CH:14]=[CH:13][C:12]([CH3:15])=[CH:11][CH:10]=1.C(=O)([O-])[O-].[K+].[K+].[CH3:22][O:23][CH2:24][CH2:25]Br>CN(C)C=O>[NH2:1][C:2]1[N:6]([CH3:7])[N:5]=[C:4]([O:8][CH2:25][CH2:24][O:23][CH3:22])[C:3]=1[C:9]1[CH:14]=[CH:13][C:12]([CH3:15])=[CH:11][CH:10]=1
参加物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 11430Potassium CarbonateHCID 809722-Bromoethyl methyl etherHCID 1784239155-amino-1-methyl-4-(4-methylphenyl)-1H-pyrazol-3-ol

生成物 1

HCID 229997133-(2-methoxyethoxy)-1-methyl-4-(4-methylphenyl)-1H-pyrazol-5-ylamine収率 51.4%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

5-amino-1-methyl-4-(4-methylphenyl)-1H-pyrazol-3-ol (Preparation 11) (305 mg) was dissolved in dimethylformamide (2 ml), potassium carbonate (622 mg) and 2-bromoethyl methyl ether (208 mg) were added. The reaction was stirred at room temperature for 1.5 hours and then at 50° C. for 12 hours. The solvent was removed under reduced pressure. The crude product was purified on silica (10 g) eluted with a solvent gradient of pentane:ethyl acetate (1:0 to 0:1) to yield the title compound as a white solid (201 mg).

後処理

  1. waitat 50° C. for 12 hours
  2. customThe solvent was removed under reduced pressure
  3. customThe crude product was purified on silica (10 g)
  4. washeluted with a solvent gradient of pentane:ethyl acetate (1:0 to 0:1)

出典と根拠

ORDレコード
ord-ef7eb5ffd8b94f339321beb9876bceb8
出典データセット
uspto-grants-2003_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06610518B2

反応ノート

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