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2-Isocyanato-1-methoxy-4-methylbenzene → 3-(2-Methoxy-5-methyl-phenyl)-1-methyl-1-pyrazin-2-yl-urea

HRID 1830757
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HRID 1830757 반응식
[CH3:1][NH:2][C:3]1[CH:8]=[N:7][CH:6]=[CH:5][N:4]=1.[CH3:9][O:10][C:11]1[CH:16]=[CH:15][C:14]([CH3:17])=[CH:13][C:12]=1[N:18]=[C:19]=[O:20].CCOC(C)=O.CCCCCC.C(Cl)Cl.CO>ClC(Cl)C>[CH3:9][O:10][C:11]1[CH:16]=[CH:15][C:14]([CH3:17])=[CH:13][C:12]=1[NH:18][C:19](=[O:20])[N:2]([CH3:1])[C:3]1[CH:8]=[N:7][CH:6]=[CH:5][N:4]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 41415202-Isocyanato-1-methoxy-4-methylbenzeneHCID 16767478N-Methylpyrazin-2-amineHCID 21226129Dichloromethane methanolHCID 21226206Ethyl acetate hexane

생성물 1

HCID 220464313-(2-Methoxy-5-methyl-phenyl)-1-methyl-1-pyrazin-2-yl-urea

시약·촉매·용매 1

HCID 6365
1,1-Dichloroethane
용매

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온도
80 °C

실험 절차

To a 0.3 M stirred solution of 2-methylaminopyrazine (1 equiv.) in dichloroethane at room temperature under nitrogen was added 2-methoxy-5-methylphenylisocyanate (1 equiv.). The reaction was warmed to 80° C. overnight and then cooled to room temperature. In most cases, the product precipitated and was isolated by filtration. Alternatively the product could be isolated by silica gel chromatography using EtOAc/hexane or CH2Cl2/MeOH as eluant. 1H-NMR (400 MHz, CDCl3) δ8.57 (s, 1H), 8.32 (s, 1H), 8.31 (s, 1H), 8.17 (s, 1H), 6.80 (i, 2H), 3.90 (s, 3H), 3.56 (s, 3H), 2.32 (s, 3H). LRMS (ESI, Positive) m/e 273.2 (M+1).

후처리

  1. temperaturecooled to room temperature
  2. customIn most cases, the product precipitated
  3. customwas isolated by filtration
  4. customAlternatively the product could be isolated by silica gel chromatography

출처 및 근거

ORD 기록
ord-7757c99411094b4eafe7b8902b065176
출처 데이터셋
uspto-grants-2006_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07067506B2

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