Potassium Carbonate → HCID 18349617、化合物

HRID 1956850ノート

反応式

HRID 1956850 の反応式
Br[CH2:2][C:3]([O:5][CH3:6])=[O:4].[Cl:7][C:8]1[CH:25]=[CH:24][C:11]([O:12][CH2:13][CH2:14][NH:15][CH2:16][CH2:17][CH2:18][N:19]2[CH:23]=[CH:22][N:21]=[CH:20]2)=[CH:10][CH:9]=1.C(=O)([O-])[O-].[K+].[K+]>CC(C)=O.CCOCC>[Cl:7][C:8]1[CH:9]=[CH:10][C:11]([O:12][CH2:13][CH2:14][N:15]([CH2:16][CH2:17][CH2:18][N:19]2[CH:23]=[CH:22][N:21]=[CH:20]2)[CH2:2][C:3]([O:5][CH3:6])=[O:4])=[CH:24][CH:25]=1

参加物

6

反応物 3

HCID 11430Potassium CarbonateHCID 60984Methyl bromoacetateHCID 18349584N-[2-(4-chlorophenoxy)ethyl]-3-(imidazol-1-yl)propylamine

生成物 1

HCID 18349617HCID 18349617、化合物

試薬・触媒・溶媒 2

HCID 180Acetone溶媒HCID 3283Diethyl Ether溶媒

実験手順

Methyl bromoacetate (2.1 g) was added to a stirred mixture of N-[2-(4-chlorophenoxy)ethyl]-3-(imidazol-1-yl)propylamine (3.87 g) and anhydrous potassium carbonate (5.73 g) in dry acetone (180 ml). The mixture was stirred and boiled under reflux for 7 hours, then left to stand at ambient temperature for 18 hours then hot filtered. The filtrate was evaporated to dryness and the residue was purified by chromatography on silica using ethyl acetate/triethylamine, 9 to 1 as the mobile phase. The product was obtained as an oil which was dissolved in ether, and extracted into 5M hydrochloric acid. The acid extracts were basified with 5M sodium hydroxide solution and the product extracted into ether to give methyl N-[2-(4-chlorophenoxy)ethyl]-N-[3-(imidazol-1-yl)propyl]glycinate as an oil.

後処理

  1. temperatureunder reflux for 7 hours
  2. waitleft
  3. customThe filtrate was evaporated to dryness
  4. customthe residue was purified by chromatography on silica
  5. customThe product was obtained as an oil which
  6. extractionextracted into 5M hydrochloric acid
  7. extractionthe product extracted into ether

出典と根拠

ORDレコード
ord-b74653787e5a45cab88a53a6a5af6672
出典データセット
uspto-grants-1998_07
特許番号
US05780642

反応ノート

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