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

HRID 1155563ノート

反応式

HRID 1155563 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)-pyridazine-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-7bcde3e3ce6d42108fe77152f282d7e6
出典データセット
uspto-grants-1981_11
特許番号
US04302587

反応ノート

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