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

HRID 1291337
ノート
印刷プレビュー

反応式

HRID 1291337 の反応式
[CH3:1][N:2]1[C:11](=[O:12])[C:10]2[C:5](=[CH:6][CH:7]=[CH:8][C:9]=2[CH3:13])[N:4]=[C:3]1[SH:14].Br[CH2:16][C:17]1[CH:32]=[CH:31][C:20]([C:21]([C:23]2[CH:28]=[CH:27][C:26]([CH2:29]Br)=[CH:25][CH:24]=2)=[O:22])=[CH:19][CH:18]=1.[CH3:33][N:34]1[CH2:39][CH2:38][NH:37][CH2:36][CH2:35]1.[OH-].[Na+].O>CN(C=O)C>[CH3:1][N:2]1[C:11](=[O:12])[C:10]2[C:5](=[CH:6][CH:7]=[CH:8][C:9]=2[CH3:13])[N:4]=[C:3]1[S:14][CH2:16][C:17]1[CH:32]=[CH:31][C:20]([C:21](=[O:22])[C:23]2[CH:28]=[CH:27][C:26]([CH2:29][N:37]3[CH2:38][CH2:39][N:34]([CH3:33])[CH2:35][CH2:36]3)=[CH:25][CH:24]=2)=[CH:19][CH:18]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 531671-MethylpiperazineHCID 23039244,4'-Bis(bromomethyl)benzophenoneHCID 23719242Sodium hydroxide--water (1/1/1)HCID 178424003HCID 178424003、化合物

生成物 1

HCID 189192153,5-Dimethyl-2-[4-[4-(4-methylpiperazinylmethyl)benzoyl]benzylthio]-4(3H)-quinazolinone

試薬・触媒・溶媒 1

HCID 6228
Dimethylformamide
溶媒

実験手順

A solution of 3,5-dimethyl-2-mercapto-4(3H)quinazolinone (1.03 g), 4,4'-bis (bromomethyl)benzophenone (1.75 g), N-methylpiperazine (500 ml) and 1N-sodium hydroxide/water (5.5 ml) in DMF (35 ml) was stirred at room temperature for 30 minutes. This reaction mixture was concentrated and the residue was dissolved in ethyl acetate, washed with water, dried, and concentrated. The residue was purified by silica gel column chromatography (chloroform: methanol: aqueous ammonia=40:1:0.1) to provide the title compound as colorless amorphous solid (180 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. concentrationconcentrated
  6. customThe residue was purified by silica gel column chromatography (chloroform: methanol: aqueous ammonia=40:1:0.1)

出典と根拠

ORDレコード
ord-fb53c5ba18e7453daecae87886e0d79c
出典データセット
uspto-grants-1998_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05753664

反応ノート

読み込み中…

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