Formamidine acetate → 6-(N,N-Dimethylamino)-3H-pyrido[3,4-d]pyrimidin-4-one

HRID 566383노트

반응식

HRID 566383 반응식
[NH2:1][C:2]1[C:3]([C:11]([OH:13])=O)=[CH:4][C:5]([N:8]([CH3:10])[CH3:9])=[N:6][CH:7]=1.C(O)(=O)C.[CH:18](N)=[NH:19]>C(O)(=O)C>[CH3:10][N:8]([C:5]1[N:6]=[CH:7][C:2]2[N:1]=[CH:18][NH:19][C:11](=[O:13])[C:3]=2[CH:4]=1)[CH3:9]

참가 물질

4

반응물 2

HCID 160693Formamidine acetateHCID 227274305-Amino-2-(dimethylamino)isonicotinic acid

생성물 1

HCID 1358174466-(N,N-Dimethylamino)-3H-pyrido[3,4-d]pyrimidin-4-one수율 44.1%

시약·촉매·용매 1

HCID 176Acetic Acid용매

실험 절차

5-Amino-2-(N,N-dimethylamino)-pyridine-4-carboxylic acid (0.54 g) was treated with formamidine acetate (3.12 g) in glacial acetic acid (20 ml) and heated at reflux for 16 hours. The mixture was cooled, evaporated to dryness in vacuo and partitioned between ethyl acetate and water. The organic phase was separated, dried over magnesium sulphate and concentrated in vacuo to give, after chromatography on silica, the title compound (0.25 g); δH CDCl3 9.10(1H,d), 8.80(1H,s), 8.31(1H,s), 7.07(1H,s), 3.20(6H,s); m/z (M+1+)191.

후처리

  1. temperatureheated
  2. temperatureat reflux for 16 hours
  3. temperatureThe mixture was cooled
  4. customevaporated to dryness in vacuo
  5. custompartitioned between ethyl acetate and water
  6. customThe organic phase was separated
  7. dry with materialdried over magnesium sulphate
  8. concentrationconcentrated in vacuo
  9. customto give

출처 및 근거

ORD 기록
ord-7f8ce20c188d414f818cf5e9796d00aa
출처 데이터셋
uspto-grants-2001_01
특허 번호
US06174889B1

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