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llms.txt · MCPガイドプライバシーポリシー · 利用規約 · サポートv1.8.0
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Malononitrile → HCID 18319895、化合物

HRID 1699359
ノート
印刷プレビュー

反応式

HRID 1699359 の反応式
[OH-].[Na+].[C:3](#[N:7])[CH2:4][C:5]#[N:6].Cl.[CH3:9][O:10][C:11]1[CH:16]=[CH:15][C:14]([C:17](=O)[CH:18]([NH2:20])[CH3:19])=[CH:13][CH:12]=1.C(#N)C(CC#N)O>O.C(O)C>[NH2:6][C:5]1[NH:20][C:18]([CH3:19])=[C:17]([C:14]2[CH:15]=[CH:16][C:11]([O:10][CH3:9])=[CH:12][CH:13]=2)[C:4]=1[C:3]#[N:7]
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 8010MalononitrileHCID 14798Sodium Hydroxide2 回HCID 126265652-Amino-1-(4-methoxyphenyl)propan-1-one hydrochlorideHCID 212535622-Hydroxybutanedinitrile

生成物 1

HCID 18319895HCID 18319895、化合物収率 63.1%

試薬・触媒・溶媒 2

HCID 702Ethanol
溶媒
HCID 962Water溶媒2 回

実験手順

To a refluxing solution (150 mL) of ethanol and water (7/3), NaOH (2.2 g, 55 mmol) and malononitrile (2.64 g, 40 mmol) were added. Then 4′-methoxy-2-aminopropiophenone hydrochloride (5.9 g, 27.2 mmol) was added in several portions. After the solution was refluxed for 30 minutes., additional malonitrile (1.3 g, 20 mmol) and NaOH (1.1 g, 27.5 mmol) were added. It was refluxed for additional 30 minutes and then poured into water (100 mL) which resulted in a precipitation. It was then filtered and washed with water until no color was washed out. The solid was then dried under vacuum at 50° C. overnight to give 2-amino-3-cyano-4-(4-methoxyphenyl)-5-methylpyrrole, (3.9 g, 63%). MS: 228 (MH+).

後処理

  1. temperatureAfter the solution was refluxed for 30 minutes
  2. temperatureIt was refluxed for additional 30 minutes
  3. customresulted in a precipitation
  4. filtrationIt was then filtered
  5. washwashed with water until no color
  6. washwas washed out
  7. customThe solid was then dried under vacuum at 50° C. overnight

出典と根拠

ORDレコード
ord-8a4db3ceffb44f70ab945eaee80cfba7
出典データセット
uspto-grants-2002_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06346534B1

反応ノート

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