Potassium Carbonate → N-(1-(2-(3,4-dimethoxyphenyl)ethyl)pyrrolidin-3-yl)phthalimide

HRID 1769673ノート

反応式

HRID 1769673 の反応式
Cl.[NH:2]1[CH2:6][CH2:5][CH:4]([N:7]2[C:11](=[O:12])[C:10]3=[CH:13][CH:14]=[CH:15][CH:16]=[C:9]3[C:8]2=[O:17])[CH2:3]1.[CH3:18][O:19][C:20]1[CH:21]=[C:22]([CH2:28][CH2:29]Cl)[CH:23]=[CH:24][C:25]=1[O:26][CH3:27].C(=O)([O-])[O-].[K+].[K+]>C(#N)C>[CH3:18][O:19][C:20]1[CH:21]=[C:22]([CH2:28][CH2:29][N:2]2[CH2:6][CH2:5][CH:4]([N:7]3[C:11](=[O:12])[C:10]4=[CH:13][CH:14]=[CH:15][CH:16]=[C:9]4[C:8]3=[O:17])[CH2:3]2)[CH:23]=[CH:24][C:25]=1[O:26][CH3:27]

参加物

5

反応物 3

HCID 11430Potassium CarbonateHCID 30153594-(2-Chloroethyl)-1,2-dimethoxybenzeneHCID 22926344N-(3-pyrrolidyl)phthalimide hydrochloride

生成物 1

HCID 15045352N-(1-(2-(3,4-dimethoxyphenyl)ethyl)pyrrolidin-3-yl)phthalimide収率 11.3%

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

6.03 g of the hydrochloride was suspended into 100 ml of acetonitrile, to which 4.79 g of 2-(3,4-dimethoxyphenyl) ethyl chloride, 8.24 g of anhydrous potassium carbonate and n-tetrabutyl ammonium iodide (catalytic amount) were added and refluxed under heating for 20 hours. After allowing them to cool, the inorganic salts were filtered out and the solvent was distilled off. After adding ethyl acetate and washed with water, they were dried with anhydrous magnesium sulfate. The solvent was concentrated and purified on silica gel chromatography to obtain 1.03 g of the above-captioned compound (total yield: 6.5%).

後処理

  1. additionwere added
  2. temperaturerefluxed
  3. temperatureunder heating for 20 hours
  4. temperatureto cool
  5. filtrationthe inorganic salts were filtered out
  6. distillationthe solvent was distilled off
  7. additionAfter adding ethyl acetate
  8. washwashed with water, they
  9. dry with materialwere dried with anhydrous magnesium sulfate
  10. concentrationThe solvent was concentrated
  11. custompurified on silica gel chromatography

出典と根拠

ORDレコード
ord-180d4a7525fb4ae28ad4a76e9d80037b
出典データセット
uspto-grants-1995_01
特許番号
US05382595

反応ノート

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