Potassium Carbonate → HCID 18349617, 화합물

HRID 378613노트

반응식

HRID 378613 반응식
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

참가 물질

6

반응물 3

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

생성물 1

HCID 18349617HCID 18349617, 화합물

시약·촉매·용매 2

HCID 180Acetone용매HCID 3283Diethyl Ether용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-70beb7a9859447858598999c5834ff18
출처 데이터셋
uspto-grants-2000_02
특허 번호
US06031109

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