Dimethylformamide → 6-[(E)-2-(dimethylamino)vinyl]-5-nitropyrimidine-2,4-diol

HRID 1615588

反応式

HRID 1615588 の反応式
[CH3:1][C:2]1[NH:7][C:6](=[O:8])[NH:5][C:4](=[O:9])[C:3]=1[N+:10]([O-:12])=[O:11].[CH3:13][N:14]([CH3:17])[CH:15]=O>>[CH3:13][N:14]([CH3:17])/[CH:15]=[CH:1]/[C:2]1[NH:7][C:6](=[O:8])[NH:5][C:4](=[O:9])[C:3]=1[N+:10]([O-:12])=[O:11]

参加物

3

反応物 2

HCID 6228DimethylformamideHCID 855236-Methyl-5-nitrouracil

生成物 1

HCID 58161886-[(E)-2-(dimethylamino)vinyl]-5-nitropyrimidine-2,4-diol収率 66%

実験手順

The procedure was adapted from that reported J. Org. Chem. 1978, 43, 2536. Dimethylfomamide-dimethyl acetal (4 mL, 30.05 mmol) was added to a warmed) (80° suspension of 6-methyl-5-nitropyrimidine-2,4(1H,3H)-dione (3 g, 17.54 mmol) in dimethylformamide (10 ml). The resultant mixture was heated to 140° for 30 min then allowed to cool to room temperature. The solid was collected by filtration and washed with ethyl acetate then dried in vacuo to afford 6-[(e)-2-(dimethylamino)vinyl]-5-nitropyrimidine-2,4(1H,3H)-dione (2.62 g, 66%).

後処理

  1. temperaturea warmed) (
  2. filtrationThe solid was collected by filtration
  3. washwashed with ethyl acetate
  4. customthen dried in vacuo

出典と根拠

ORDレコード
ord-2ca71096589b41558dd49c34a5b7f392
出典データセット
uspto-grants-2014_07
特許番号
US08765755B2

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