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4,6-Dichloroquinazoline → 4-(4-Chloro-3-nitrobenzyl)amino-6-chloroquinazoline

HRID 1003504
ノート
印刷プレビュー

反応式

HRID 1003504 の反応式
Cl[C:2]1[C:11]2[C:6](=[CH:7][CH:8]=[C:9]([Cl:12])[CH:10]=2)[N:5]=[CH:4][N:3]=1.Cl.[Cl:14][C:15]1[CH:22]=[CH:21][C:18]([CH2:19][NH2:20])=[CH:17][C:16]=1[N+:23]([O-:25])=[O:24]>C(O)(C)C.C(N(CC)CC)C>[Cl:14][C:15]1[CH:22]=[CH:21][C:18]([CH2:19][NH:20][C:2]2[C:11]3[C:6](=[CH:7][CH:8]=[C:9]([Cl:12])[CH:10]=3)[N:5]=[CH:4][N:3]=2)=[CH:17][C:16]=1[N+:23]([O-:25])=[O:24]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 2

HCID 2460244,6-DichloroquinazolineHCID 18796739(4-Chloro-3-nitrobenzyl)amine hydrochloride

生成物 1

HCID 187967424-(4-Chloro-3-nitrobenzyl)amino-6-chloroquinazoline収率 92.6%

試薬・触媒・溶媒 2

HCID 3776Isopropanol溶媒HCID 8471Triethylamine溶媒

実験手順

3.00 g (0.015 mol) of 4,6-dichloroquinazoline and 3.80 g (0.0170 mol) of 4-chloro-3-nitrobenzylamine hydrochloride were dissolved in a mixture comprising 100 ml of isopropyl alcohol and 15 ml of triethylamine. The obtained solution was heated under reflux for 24 hours and distilled under a reduced pressure to remove the solvent. The residue was purified by silica gel column chromatography (chloroform/ethyl acetate) and recrystallized from chloroform/n-hexane to give 4.85 g of the title compounds as a pale-yellow crystal.

後処理

  1. temperatureThe obtained solution was heated
  2. temperatureunder reflux for 24 hours
  3. distillationdistilled under a reduced pressure
  4. customto remove the solvent
  5. customThe residue was purified by silica gel column chromatography (chloroform/ethyl acetate)
  6. customrecrystallized from chloroform/n-hexane

出典と根拠

ORDレコード
ord-7b20296534634a0fb0e54809962b9824
出典データセット
uspto-grants-2000_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06046206

反応ノート

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