Methyl pyruvate → 5,7-diamino-1,3-dimethylpyrimido(4,5-c)pyridazin-4(1H)-one

HRID 127190ノート

反応式

HRID 127190 の反応式
[NH2:1][C:2]1[N:7]=[C:6]([NH2:8])[CH:5]=[C:4]([N:9]([CH3:11])[NH2:10])[N:3]=1.[C:12](OC)(=[O:16])[C:13]([CH3:15])=O>CO>[NH2:8][C:6]1[C:5]2[C:12](=[O:16])[C:13]([CH3:15])=[N:10][N:9]([CH3:11])[C:4]=2[N:3]=[C:2]([NH2:1])[N:7]=1

参加物

4

反応物 2

HCID 11748Methyl pyruvateHCID 124630642,4-Diamino-6-(1-methylhydrazino)pyrimidine

生成物 1

HCID 124630735,7-diamino-1,3-dimethylpyrimido(4,5-c)pyridazin-4(1H)-one収率 76%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

To a refluxing solution of 2,4-diamino-6-(1-methylhydrazino)-pyrimidine (500 mg) in anhydrous methanol (15 ml) was added methyl pyruvate (496 mg) over a five minute period. Reflux was continued for 5 hours after which time the solid which had separated was collected by suction filtration of the hot mixture, washed with methanol, and dried under vacuum at 70° C. to yield tan crystals of 5,7-diamino-1,3-dimethylpyrimido [4,5-c]pyridazin-4(1H)-one (508 mg; 76% of theoretical yield; M.P.>275° C.)

後処理

  1. temperatureReflux
  2. customafter which time the solid which had separated
  3. filtrationwas collected by suction filtration of the hot mixture
  4. washwashed with methanol
  5. customdried under vacuum at 70° C.

出典と根拠

ORDレコード
ord-74efd690c2284a6fbbca81fd2e226350
出典データセット
uspto-grants-1981_03
特許番号
US04255427

反応ノート

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