Water → 3-(4,6-Dimethoxypyrimidine-2-yl)-2-methyl-7-metoxymethylindole

HRID 1163449ノート

反応式

HRID 1163449 の反応式
[CH3:1][O:2][C:3]1[CH:8]=[C:7]([O:9][CH3:10])[N:6]=[C:5]([CH2:11][C:12](=O)[CH3:13])[N:4]=1.[CH3:15][O:16][CH2:17][C:18]1[CH:23]=[CH:22][CH:21]=[CH:20][C:19]=1[NH:24]N.C1(C)C=CC=CC=1.O>[Cl-].[Zn+2].[Cl-].C(OCC)(=O)C>[CH3:1][O:2][C:3]1[CH:8]=[C:7]([O:9][CH3:10])[N:6]=[C:5]([C:11]2[C:20]3[C:19](=[C:18]([CH2:17][O:16][CH3:15])[CH:23]=[CH:22][CH:21]=3)[NH:24][C:12]=2[CH3:13])[N:4]=1

参加物

7

反応物 4

HCID 962WaterHCID 1140TolueneHCID 112640521-(4,6-Dimethoxypyrimidin-2-yl)propan-2-oneHCID 129793652-Methoxymethylphenylhydrazine

生成物 1

HCID 115732153-(4,6-Dimethoxypyrimidine-2-yl)-2-methyl-7-metoxymethylindole収率 46.2%

試薬・触媒・溶媒 2

HCID 3007855Zincchloride触媒HCID 8857Ethyl Acetate溶媒

実験手順

Into a reactor were fed 6.2 g (31.6 m moles) of 1-(4,6-dimethoxypyrimidine-2-yl)-2-propanone, 4.8 g (31.5 m moles) of 2-methoxymethylphenylhydrazine, 4.76 g (34.9 m moles) of zinc chloride and 60 ml of toluene. Refluxing was made for 2 hours with heating. After the completion of the reaction, the reaction mixture was cooled to room temperature. Water and ethyl acetate were added and phase separation was made. The ethyl acetate layer was concentrated. The resulting crystals were washed with diisopropyl ether to obtain 4.57 g (14.6 m moles) of 3-(4,6-dimethoxypyrimidine-2-yl)-2-methyl-7-metoxymethylindole. Yield: 46%,

後処理

  1. customInto a reactor were fed
  2. temperatureRefluxing
  3. temperaturewith heating
  4. customAfter the completion of the reaction
  5. customphase separation
  6. concentrationThe ethyl acetate layer was concentrated
  7. washThe resulting crystals were washed with diisopropyl ether

出典と根拠

ORDレコード
ord-060df879c94b46de93f332e095a23838
出典データセット
uspto-grants-2010_10
特許番号
US07820861B2

反応ノート

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