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

HRID 1246229

반응식

HRID 1246229 반응식
[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

참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 31374Dimethylacetamide용매

반응 조건

온도
40 °C

실험 절차

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)

후처리

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

출처 및 근거

ORD 기록
ord-ce5fd100c500424b86166da2397c6b45
출처 데이터셋
uspto-grants-2006_10
특허 번호
US07125993B2

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