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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
ノート
印刷プレビュー

反応式

HRID 1516834 の反応式
[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
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

3

反応物 1

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

反応条件

温度
65 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-fbf38190112b4f2c9343b38e4a117a90
出典データセット
uspto-grants-2012_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08227601B2

反応ノート

読み込み中…

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