Potassium Carbonate → HCID 22326840, 화합물

HRID 495463노트

반응식

HRID 495463 반응식
Cl[CH2:2][CH2:3][O:4][C:5]1[CH:10]=[CH:9][C:8]([N+:11]([O-:13])=[O:12])=[CH:7][C:6]=1[O:14][CH3:15].[CH3:16][N:17]1[CH2:22][CH2:21][NH:20][CH2:19][CH2:18]1.C([O-])([O-])=O.[K+].[K+]>CC#N>[CH3:15][O:14][C:6]1[CH:7]=[C:8]([N+:11]([O-:13])=[O:12])[CH:9]=[CH:10][C:5]=1[O:4][CH2:3][CH2:2][N:20]1[CH2:21][CH2:22][N:17]([CH3:16])[CH2:18][CH2:19]1

참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 531671-MethylpiperazineHCID 22326897HCID 22326897, 화합물

생성물 1

HCID 22326840HCID 22326840, 화합물

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

A mixture of 1-(2-chloroethoxy)-2-methoxy-4-nitrobenzene (Step A, 1 eq), N-methylpiperazine (3 eq) and K2CO3 (2.5 eq) in CH3CN was stirred and heated under reflux until HPLC indicated the reaction was complete. The resulting solid was filtered, rinsed well with CH2Cl2 and the filtrate and washings were combined, concentrated and purified by column chromatography giving 1-[2-(2-methoxy-4-nitro-phenoxy)-ethyl]-4-methyl-piperazine.

후처리

  1. temperatureheated
  2. temperatureunder reflux until HPLC
  3. filtrationThe resulting solid was filtered
  4. washrinsed well with CH2Cl2
  5. concentrationconcentrated
  6. custompurified by column chromatography

출처 및 근거

ORD 기록
ord-7751c82824fa4fd3a6a4caa84299b606
출처 데이터셋
uspto-grants-2005_09
특허 번호
US06939874B2

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