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Formic Acid → 2,5-Diethyl-7-(4-methyl-1-piperazinyl)-1,2,4-triazolo[1,5-c]pyrimidine

HRID 1589635
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HRID 1589635 반응식
[CH2:1]([C:3]1[N:7]2[C:8]([CH2:19][CH3:20])=[N:9][C:10]([N:12]3[CH2:17][CH2:16][N:15]([CH3:18])[CH2:14][CH2:13]3)=[CH:11][C:6]2=[N:5][N:4]=1)[CH3:2].C(O)=O.C(=O)(O)[O-].[Na+]>O>[CH2:1]([C:3]1[N:7]=[C:6]2[N:5]([C:8]([CH2:19][CH3:20])=[N:9][C:10]([N:12]3[CH2:17][CH2:16][N:15]([CH3:18])[CH2:14][CH2:13]3)=[CH:11]2)[N:4]=1)[CH3:2]
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참가 물질

5

반응물 3

HCID 284Formic AcidHCID 516892Sodium BicarbonateHCID 13393635HCID 13393635, 화합물

생성물 1

HCID 135662412,5-Diethyl-7-(4-methyl-1-piperazinyl)-1,2,4-triazolo[1,5-c]pyrimidine

시약·촉매·용매 1

HCID 962Water용매

실험 절차

A mixture of 3.3 g of 3,5-diethyl-7-(4-methyl-1-piperazinyl)-1,2,4-triazolo[4,3-c]pyrimidine and 50 ml of 97% formic acid was heated at reflux for 18 hours. The mixture was cooled and evaporated in vacuo to provide a residue which was diluted with 100 ml of water and carefully neutralized with sodium bicarbonate. The solution was extracted with chloroform. The extracts were dried and then concentrated to provide an oil which solidified and was collected by filtration, washed with water and dried. Recrystallization from hexane provided off-white crystalline solid 2,5-diethyl-7-(4-methyl-1-piperazinyl)-1,2,4-triazolo[1,5-c]pyrimidine, m.p. 87°-88° C. Analysis: Calculated for C14H22N6 : %C, 61.3; %H, 8.1; %N, 30.6; Found: %C, 60.6; %H, 8.1, %N, 30.6. The structural assignment was confirmed by infrared and nuclear magnetic resonance spectral analyses.

후처리

  1. temperaturewas heated
  2. temperatureat reflux for 18 hours
  3. temperatureThe mixture was cooled
  4. customevaporated in vacuo
  5. customto provide a residue which
  6. extractionThe solution was extracted with chloroform
  7. customThe extracts were dried
  8. concentrationconcentrated
  9. customto provide an oil which
  10. filtrationwas collected by filtration
  11. washwashed with water
  12. customdried
  13. customRecrystallization from hexane provided off-white crystalline solid 2,5-diethyl-7-(4-methyl-1-piperazinyl)-1,2,4-triazolo[1,5-c]pyrimidine, m.p. 87°-88° C

출처 및 근거

ORD 기록
ord-ef815fc0c9124fa19f4e1545c9fa8330
출처 데이터셋
uspto-grants-1986_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04572910

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