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Aminopyrazine → HCID 22046313, 화합물

HRID 1821731
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HRID 1821731 반응식
[CH3:1][O:2][C:3]1[CH:8]=[C:7]([N+:9]([O-:11])=[O:10])[CH:6]=[CH:5][C:4]=1[N:12]=[C:13]=[O:14].[NH2:15][C:16]1[CH:21]=[N:20][CH:19]=[CH:18][N:17]=1>C1COCC1>[CH3:1][O:2][C:3]1[CH:8]=[C:7]([N+:9]([O-:11])=[O:10])[CH:6]=[CH:5][C:4]=1[NH:12][C:13]([NH:15][C:16]1[CH:21]=[N:20][CH:19]=[CH:18][N:17]=1)=[O:14]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 78747AminopyrazineHCID 34920221-Isocyanato-2-methoxy-4-nitrobenzene

생성물 1

HCID 22046313HCID 22046313, 화합물

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

A mixture of 2-methoxy-4-nitrophenyl isocyanate (15.0 g, 77 mmol) and aminopyrazine (7.35 g, 77 mmol) in THF (600 mL) was stirred at reflux for 24 hours. The product precipitated from the cooled reaction mixture and was collected by filtration, washed with ethyl acetate, triturated with hot ethanol, and dried in vacuo (16.3 g, 73%). 1H NMR (300 Mhz, d6DMSO) δ: 10.50 (br s, 1H), 10.42 (s, 1H), 8.94 (s, 1H), 8.48 (d, 1H), 8.39 (s, 1H), 8.32 (d, 1H), 7.95 (dd, J=9.1, 2.4 Hz, 1H), 7.84 (d, J=2.4 Hz, 1H), 4.08 (s, 3H).

후처리

  1. temperatureat reflux for 24 hours
  2. customThe product precipitated from the cooled reaction mixture
  3. filtrationwas collected by filtration
  4. washwashed with ethyl acetate
  5. customtriturated with hot ethanol
  6. customdried in vacuo (16.3 g, 73%)

출처 및 근거

ORD 기록
ord-f4b516cb60bd482e9266b87419b5639e
출처 데이터셋
uspto-grants-2009_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07608618B2

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