Methyl iodide → 8-Ethyl-4-methyl-4H-pyrazolo[4',3':5,6]pyrido[3,4-e][1,2,4]triazolo[1,5-a]pyrimidin-5(8H)-one

HRID 2287144노트

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HRID 2287144 반응식
[CH2:1]([N:3]1[C:7]2[N:8]=[CH:9][C:10]3[C:11](=[O:19])[NH:12][C:13]4[N:14]([N:16]=[CH:17][N:18]=4)[C:15]=3[C:6]=2[CH:5]=[N:4]1)[CH3:2].[Na].[CH3:21]I>COCCOCCOC>[CH2:1]([N:3]1[C:7]2[N:8]=[CH:9][C:10]3[C:11](=[O:19])[N:12]([CH3:21])[C:13]4[N:14]([N:16]=[CH:17][N:18]=4)[C:15]=3[C:6]=2[CH:5]=[N:4]1)[CH3:2]

참가 물질

5

반응물 3

HCID 6328Methyl iodideHCID 5360545SodiumHCID 1355938528-Ethyl-4H-pyrazolo[4',3':5,6]pyrido[3,4-e][1,2,4]-triazolo[1,5-a]pyrimidin-5(8H)-one

생성물 1

HCID 234596128-Ethyl-4-methyl-4H-pyrazolo[4',3':5,6]pyrido[3,4-e][1,2,4]triazolo[1,5-a]pyrimidin-5(8H)-one

시약·촉매·용매 1

HCID 8150Diglyme용매

실험 절차

2.6 g. of 8-ethyl-4H-pyrazolo[4',3':5,6]pyrido[3,4-e][1,2,4]triazolo[1,5-a]pyrimidin-5(8H)-one (0.01 mol.) are treated with 0.3 g. of sodium in 50 ml. of diethyleneglycol dimethyl ether at reflux temperature with stirring for 30 minutes. After this time, the temperature is lowered to 60° and 3 g. of methyl iodide are added. Stirring and heating is continued for 12 hours. The precipitate of sodium iodide is filtered off and the solvent distilled from the mother liquor. The remaining 8ethyl-4-methyl-4Hpyrazolo[4',3':5,6]pyrido[3,4-e][1,2,4]triazolo[1,5-a]pyrimidin5(8H)-one is recrystallized from butanol, yield 2 g. (75%); m.p. 208°-210°.

후처리

  1. customis lowered to 60°
  2. stirringStirring
  3. temperatureheating
  4. waitis continued for 12 hours
  5. filtrationThe precipitate of sodium iodide is filtered off
  6. distillationthe solvent distilled from the mother liquor
  7. customThe remaining 8ethyl-4-methyl-4Hpyrazolo[4',3':5,6]pyrido[3,4-e][1,2,4]triazolo[1,5-a]pyrimidin5(8H)-one is recrystallized from butanol, yield 2 g

출처 및 근거

ORD 기록
ord-0ce8de9a43a047ce93dfd1a791f33d79
출처 데이터셋
uspto-grants-1981_05
특허 번호
US04269836

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