Potassium Carbonate → HCID 22326840、化合物

HRID 495463ノート

反応式

HRID 495463 の反応式
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

参加物

5

反応物 3

HCID 11430Potassium CarbonateHCID 531671-MethylpiperazineHCID 22326897HCID 22326897、化合物

生成物 1

HCID 22326840HCID 22326840、化合物

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-7751c82824fa4fd3a6a4caa84299b606
出典データセット
uspto-grants-2005_09
特許番号
US06939874B2

反応ノート

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