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4-Bromophenacyl bromide → 2-Amino-5-(4-bromophenyl)pyrrole-3-carboxamide

HRID 1011565
ノート
印刷プレビュー

反応式

HRID 1011565 の反応式
[O-]CC.[Na+].[CH2:5]([C:9]([NH2:11])=[O:10])[C:6]([NH2:8])=[NH:7].Cl.Br[CH2:14][C:15]([C:17]1[CH:22]=[CH:21][C:20]([Br:23])=[CH:19][CH:18]=1)=O>C(O)C>[NH2:7][C:6]1[NH:8][C:15]([C:17]2[CH:22]=[CH:21][C:20]([Br:23])=[CH:19][CH:18]=2)=[CH:14][C:5]=1[C:9]([NH2:11])=[O:10]
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 3

HCID 74544-Bromophenacyl bromideHCID 2723922Sodium ethoxideHCID 3084595Amidinomalonamide hydrochloride

生成物 1

HCID 592859782-Amino-5-(4-bromophenyl)pyrrole-3-carboxamide収率 9%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

Under ice-cooling, sodium ethoxide (2.1 g, 30 mmol) was added to a suspension of malonamamidine hydrochloride (4.1 g, 30 mmol) in dehydrated ethanol (50 mL), and then the mixture was stirred for 20 minutes. Moreover, 2,4′-dibromoacetophenone (4.2 g, 15 mmol) was added thereto, and the whole was stirred at room temperature for 5 hours. After the insoluble solid was filtered out, the filtrate was concentrated in vacuo. The obtained residue was purified by silica gel column chromatography to give the title reference compound (0.37 g) as a black solid (Yield 9%).

後処理

  1. temperatureUnder ice-cooling
  2. stirringthe whole was stirred at room temperature for 5 hours
  3. filtrationAfter the insoluble solid was filtered out
  4. concentrationthe filtrate was concentrated in vacuo
  5. customThe obtained residue was purified by silica gel column chromatography

出典と根拠

ORDレコード
ord-b2436f09308e4ebf8d1fc7d84b09038e
出典データセット
uspto-grants-2011_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07977371B2

反応ノート

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