Dimethylformamide dimethyl acetal → N'-(3-Ethyl-2,6-dioxo-1,2,3,6-tetrahydropyrimidin-4-yl)-N,N-dimethylformimidamide

HRID 1246229

反応式

HRID 1246229 の反応式
[NH2:1][C:2]1[N:7]([CH2:8][CH3:9])[C:6](=[O:10])[NH:5][C:4](=[O:11])[CH:3]=1.CO[CH:14](OC)[N:15]([CH3:17])[CH3:16]>CN(C)C(=O)C>[CH3:14][N:15]([CH3:17])[CH:16]=[N:1][C:2]1[N:7]([CH2:8][CH3:9])[C:6](=[O:10])[NH:5][C:4](=[O:11])[CH:3]=1

参加物

4

反応物 2

HCID 78373Dimethylformamide dimethyl acetalHCID 8538996-Amino-1-ethyl-1,2,3,4-tetrahydropyrimidine-2,4-dione

生成物 1

HCID 66630127N'-(3-Ethyl-2,6-dioxo-1,2,3,6-tetrahydropyrimidin-4-yl)-N,N-dimethylformimidamide

試薬・触媒・溶媒 1

HCID 31374Dimethylacetamide溶媒

反応条件

温度
40 °C

実験手順

A suspension of 6-amino-1-ethyl-1,3-dihydropyrimidine-2,4-dione (0.77 g, 5 mmol) in anhydrous N,N-dimethylacetamide (25 ml) and N,N-dimethylformamide dimethylacetal (2.7 ml, 20 mmol) and was warmed at 40° C. for 90 minutes. Solvent was then removed under reduced pressure, and the residue triturated with ethanol, filtered, and washed with ethanol, to provide 6-[2-(dimethylamino)-1-azavinyl]-1-ethyl-1,3-dihydropyrimidine-2,4-dione, a compound of formula (6). 1H-NMR (DMSO-d6) δ 10.62 (s, 1H), 8.08 (s, 1H), 4.99 (s, 1H), 3.88–3.95 (m, 2H), 3.13 (s, 3H), 2.99 (s, 3H), 1.07 (t, 3H, J=7.03 Hz); MS m/z 210.86 (M+), 232.87 (M++Na)

後処理

  1. customSolvent was then removed under reduced pressure
  2. customthe residue triturated with ethanol
  3. filtrationfiltered
  4. washwashed with ethanol

出典と根拠

ORDレコード
ord-ce5fd100c500424b86166da2397c6b45
出典データセット
uspto-grants-2006_10
特許番号
US07125993B2

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