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N'-(1-benzyl-4-methyl-5-nitro-6-oxopyrimidin-2-yl)-N,N-dimethylmethanimidamide → N'-[1-benzyl-4-[(E)-2-(dimethylamino)ethenyl]-5-nitro-6-oxopyrimidin-2-yl]-N,N-dimethylmethanimidamide

HRID 1516834
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HRID 1516834 반응식
[CH2:1]([N:8]1[C:13](=[O:14])[C:12]([N+:15]([O-:17])=[O:16])=[C:11]([CH3:18])[N:10]=[C:9]1/[N:19]=[CH:20]/[N:21]([CH3:23])[CH3:22])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1>CN(C=O)C>[CH2:1]([N:8]1[C:13](=[O:14])[C:12]([N+:15]([O-:17])=[O:16])=[C:11](/[CH:18]=[CH:1]/[N:8]([CH3:13])[CH3:9])[N:10]=[C:9]1/[N:19]=[CH:20]/[N:21]([CH3:22])[CH3:23])[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

3

반응물 1

HCID 11186127N'-(1-benzyl-4-methyl-5-nitro-6-oxopyrimidin-2-yl)-N,N-dimethylmethanimidamide

생성물 1

HCID 15376104N'-[1-benzyl-4-[(E)-2-(dimethylamino)ethenyl]-5-nitro-6-oxopyrimidin-2-yl]-N,N-dimethylmethanimidamide

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

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온도
65 °C

실험 절차

To a solution of (E)-N′(1-benzyl-4-methyl-5-nitro-6-oxo-1,6-dihydropyrimidin-2-yl)-N,N-dimethylformimidamide (64.7 g, 0.2 mol) in DMF (254 mL) was added DMF-dimethylacetal (54.5 mL, 0.41 mol). The reaction mixture was stirred for 3 h at 65° C., cooled, and the solvent was removed under reduced pressure. The residue was triturated with ethanol, and the solid was collected by vacuum filtration (69.2 g, 91%) and used in the next step without further purification.

후처리

  1. temperaturecooled
  2. customthe solvent was removed under reduced pressure
  3. customThe residue was triturated with ethanol
  4. filtrationthe solid was collected by vacuum filtration (69.2 g, 91%)
  5. customused in the next step without further purification

출처 및 근거

ORD 기록
ord-fbf38190112b4f2c9343b38e4a117a90
출처 데이터셋
uspto-grants-2012_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08227601B2

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