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

HRID 1507790
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반응식

HRID 1507790 반응식
[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
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참가 물질

4

반응물 2

HCID 85247Trimethylsilyl iodideHCID 2986625HCID 2986625, 화합물

생성물 1

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

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

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%).

후처리

  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

출처 및 근거

ORD 기록
ord-586aae6bc31446cc9a245f7295dfe23f
출처 데이터셋
uspto-grants-2015_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09221822B2

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