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Trimethylsilyl iodide → N-(3-Methylphenyl)piperazine-1-carboxamide

HRID 1507790
ノート
印刷プレビュー

反応式

HRID 1507790 の反応式
[C:1]1([CH3:21])[CH:6]=[CH:5][CH:4]=[C:3]([NH:7][C:8]([N:10]2[CH2:15][CH2:14][N:13](C(OCC)=O)[CH2:12][CH2:11]2)=[O:9])[CH:2]=1.I[Si](C)(C)C>ClCCl>[C:1]1([CH3:21])[CH:6]=[CH:5][CH:4]=[C:3]([NH:7][C:8]([N:10]2[CH2:15][CH2:14][NH:13][CH2:12][CH2:11]2)=[O:9])[CH:2]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 85247Trimethylsilyl iodideHCID 2986625HCID 2986625、化合物

生成物 1

HCID 16769291N-(3-Methylphenyl)piperazine-1-carboxamide収率 100%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

A suspension of ethyl 4-(m-tolylcarbamoyl)piperazine-1-carboxylate (example 59, 1.5 g, 5.15 mmol) in dichloromethane (25 ml) was treated dropwise at room temperature with iodotrimethylsilane (1.6 ml, 11.3 mmol). The reaction mixture was stirred under nitrogen at room temperature overnight. The volatiles were evaporated to dryness, diluted with methanol and the solid was filtered off. The solid was washed with methanol and dichloromethane and dried under vacuum to yield the title compound as a yellow solid (1.1 g, 100%).

後処理

  1. customThe volatiles were evaporated to dryness
  2. additiondiluted with methanol
  3. filtrationthe solid was filtered off
  4. washThe solid was washed with methanol and dichloromethane
  5. customdried under vacuum

出典と根拠

ORDレコード
ord-586aae6bc31446cc9a245f7295dfe23f
出典データセット
uspto-grants-2015_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09221822B2

反応ノート

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