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Oxalyl chloride → 1-allyl-3,5-dichloro-6-methylpyrazin-2(1H)-one

HRID 361374
노트
인쇄 미리보기

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HRID 361374 반응식
[C:1]([Cl:6])(=O)[C:2](Cl)=[O:3].[ClH:7].[CH2:8]([NH:11][CH:12]([CH3:15])[C:13]#[N:14])[CH:9]=[CH2:10]>ClC1C=CC=CC=1Cl>[CH2:8]([N:11]1[C:12]([CH3:15])=[C:13]([Cl:7])[N:14]=[C:1]([Cl:6])[C:2]1=[O:3])[CH:9]=[CH2:10]
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참가 물질

4

반응물 2

HCID 65578Oxalyl chlorideHCID 86753643alpha-(Allylamino)-propionitrile hydrochloride

생성물 1

HCID 106564741-allyl-3,5-dichloro-6-methylpyrazin-2(1H)-one

시약·촉매·용매 1

HCID 72391,2-Dichlorobenzene용매

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온도
100 °C

실험 절차

A stirred mixture of oxalyl chloride (30.5 ml, 0.35 mol) and α-(allylamino)-propionitrile hydrochloride (10.26 g, 70 mmol) in o-dichlorobenzene (100 ml) was heated to 100° C. for 15 h. The solvent was evaporated in vacuo and the residual black oil was purified by flash column chromatography on silica (eluting with 30% ethyl acetate hexanes) to give the title compound as a tan crystalline solid:

후처리

  1. customThe solvent was evaporated in vacuo
  2. customthe residual black oil was purified by flash column chromatography on silica (eluting with 30% ethyl acetate hexanes)

출처 및 근거

ORD 기록
ord-929d9cd804db4288ba9afabd3d0fb51e
출처 데이터셋
uspto-grants-1999_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05866573

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