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

HRID 1155563노트

반응식

HRID 1155563 반응식
[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

참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

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.).

후처리

  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.

출처 및 근거

ORD 기록
ord-7bcde3e3ce6d42108fe77152f282d7e6
출처 데이터셋
uspto-grants-1981_11
특허 번호
US04302587

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