Water → HCID 69497924、化合物

HRID 460666ノート

反応式

HRID 460666 の反応式
[CH3:1][O:2][C:3]1[CH:15]=[CH:14][CH:13]=[CH:12][C:4]=1[CH:5]=[C:6]1[CH2:10][CH2:9][NH:8][C:7]1=[O:11].[H-].[Na+].[CH3:18][O:19][CH2:20][CH2:21]Cl.O>CN(C)C=O>[CH3:1][O:2][C:3]1[CH:15]=[CH:14][CH:13]=[CH:12][C:4]=1[CH:5]=[C:6]1[CH2:10][CH2:9][N:8]([CH2:21][CH2:20][O:19][CH3:18])[C:7]1=[O:11]

参加物

6

反応物 4

HCID 962WaterHCID 123162-Chloroethyl methyl etherHCID 24758Sodium hydrideHCID 2641593-(2'-Methoxybenzylidene)-2-pyrrolidone

生成物 1

HCID 69497924HCID 69497924、化合物

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

The intermediate 3-(2′-methoxybenzylidene)-2-pyrrolidone (5.0 g) obtained in Example 317 was dissolved in dimethylformamide (50 ml) and sodium hydride (0.99 g) was added under ice-cooling. The mixture was stirred at room temperature for 30 min. To the reaction mixture was again added 2-methoxyethyl chloride (2.3 ml) under ice-cooling, and the mixture was stirred at room temperature for 1 hr and at 70° C. for 1 hr. After cooling, the reaction mixture was poured into water and extracted with ethyl acetate. The organic layer was dried over anhydrous sodium sulfate and concentrated under reduced pressure to give an oily title compound (2.8 g).

後処理

  1. temperaturecooling
  2. temperaturecooling
  3. stirringthe mixture was stirred at room temperature for 1 hr and at 70° C. for 1 hr
  4. temperatureAfter cooling
  5. extractionextracted with ethyl acetate
  6. dry with materialThe organic layer was dried over anhydrous sodium sulfate
  7. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-2f4d75ed6b214df99216f686092b13cf
出典データセット
uspto-grants-2007_03
特許番号
US07196199B2

反応ノート

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