1-Methylpiperazine → 3,5-Dimethyl-2-[4-[4-[2-(4-methylpiperazinyl)ethoxy]benzoyl]benzylthio]-4(3H)-quinazolinone dihydrochloride

HRID 1291376ノート

反応式

HRID 1291376 の反応式
[Cl:1][CH2:2][CH2:3][O:4][C:5]1[CH:33]=[CH:32][C:8]([C:9]([C:11]2[CH:31]=[CH:30][C:14]([CH2:15][S:16][C:17]3[N:26]([CH3:27])[C:25](=[O:28])[C:24]4[C:19](=[CH:20][CH:21]=[CH:22][C:23]=4[CH3:29])[N:18]=3)=[CH:13][CH:12]=2)=[O:10])=[CH:7][CH:6]=1.[CH3:34][N:35]1[CH2:40][CH2:39][NH:38][CH2:37][CH2:36]1>CN(C=O)C>[ClH:1].[ClH:1].[CH3:27][N:26]1[C:25](=[O:28])[C:24]2[C:19](=[CH:20][CH:21]=[CH:22][C:23]=2[CH3:29])[N:18]=[C:17]1[S:16][CH2:15][C:14]1[CH:30]=[CH:31][C:11]([C:9](=[O:10])[C:8]2[CH:32]=[CH:33][C:5]([O:4][CH2:3][CH2:2][N:38]3[CH2:39][CH2:40][N:35]([CH3:34])[CH2:36][CH2:37]3)=[CH:6][CH:7]=2)=[CH:12][CH:13]=1

参加物

4

反応物 2

HCID 531671-MethylpiperazineHCID 189188132-[4-[4-(2-Chloroethoxy)benzoyl]benzylthio]-3,5-dimethyl-4(3H)-quinazolinone

生成物 1

HCID 189192263,5-Dimethyl-2-[4-[4-[2-(4-methylpiperazinyl)ethoxy]benzoyl]benzylthio]-4(3H)-quinazolinone dihydrochloride

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

A solution of 2-[4-[4-(2-chloroethoxy]benzoyl]benzylthio]-3,5-dimethyl-4(3H)-quinazolinone (173 mg) and 1-methylpiperazine (0.12 ml) in DMF (5 ml) was stirred at 100° C. for 15 hours. This reaction mixture was concentrated and the residue was dissolved in ethyl acetate, washed with water, and dried. Then, hydrogen chloride/ethyl acetate was added and the precipitated hydrochloride was collected by filtration and dried to provide the title compound as colorless solid (122 mg).

後処理

  1. concentrationThis reaction mixture was concentrated
  2. dissolutionthe residue was dissolved in ethyl acetate
  3. washwashed with water
  4. customdried
  5. additionThen, hydrogen chloride/ethyl acetate was added
  6. filtrationthe precipitated hydrochloride was collected by filtration
  7. customdried

出典と根拠

ORDレコード
ord-a1702bb215d745e1846ee33727b9a73a
出典データセット
uspto-grants-1998_05
特許番号
US05753664

反応ノート

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