Water → 5-Methyl-7-phenyl[1,2,4]triazolo[1,5-a]pyrimidin-2-amine

HRID 653573

반응식

HRID 653573 반응식
[NH2:1][C:2]1[N:6]=[C:5]([NH2:7])[NH:4][N:3]=1.[C:8]([CH2:16][C:17](=O)[CH3:18])(=O)[C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=1.C(Cl)Cl.O>C(O)(=O)C>[CH3:18][C:17]1[CH:16]=[C:8]([C:9]2[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=2)[N:3]2[N:4]=[C:5]([NH2:7])[N:6]=[C:2]2[N:1]=1

참가 물질

6

반응물 4

HCID 962WaterHCID 6344DichloromethaneHCID 7166BenzoylacetoneHCID 150783,5-Diamino-1,2,4-triazole

생성물 1

HCID 9757135-Methyl-7-phenyl[1,2,4]triazolo[1,5-a]pyrimidin-2-amine수율 100%

시약·촉매·용매 1

HCID 176Acetic Acid용매

실험 절차

A mixture of 7.0 g (71 mmol) 3,5-diamino-1,2,4-triazole and 12.0 g (74 mmol) benzoylacetone in 100 ml of glacial acetic acid was heated at reflux 2 hours. After cooling, methylene chloride (200 ml) was added followed by the addition of excess water. The organic layer was separated, washed with water, brine, dried over magensium sulfate and evaporated in vacuo to give a solid residue to which ethyl acetate was added. Filtering gave 16.0 g of crude 5-methyl-7-phenyl-1,2,4-triazolo[1,5-a]pyrimidin-2-amine (m.p. 246°-250° C.) which was used directly in the next step.

후처리

  1. temperaturewas heated
  2. temperatureat reflux 2 hours
  3. temperatureAfter cooling
  4. customThe organic layer was separated
  5. washwashed with water, brine
  6. dry with materialdried over magensium sulfate
  7. customevaporated in vacuo
  8. customto give a solid residue to which ethyl acetate
  9. additionwas added
  10. filtrationFiltering

출처 및 근거

ORD 기록
ord-d978f1943c9f42c9a878a6ac2d50f561
출처 데이터셋
uspto-grants-1992_07
특허 번호
US05127936

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