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

HRID 1704833
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HRID 1704833 반응식
[CH2:1]([N:3]1[C:7]2[N:8]=[CH:9][C:10]3[C:11](=[O:20])[NH:12][C:13]4[N:14]([N:16]=[C:17]([CH3:19])[CH:18]=4)[C:15]=3[C:6]=2[CH:5]=[N:4]1)[CH3:2].[H-].[Na+].[CH3:23]I>COCCOCCOC>[CH3:19][C:17]1[CH:18]=[C:13]2[N:12]([CH3:23])[C:11](=[O:20])[C:10]3[CH:9]=[N:8][C:7]4[N:3]([CH2:1][CH3:2])[N:4]=[CH:5][C:6]=4[C:15]=3[N:14]2[N:16]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 6328Methyl iodideHCID 24758Sodium hydrideHCID 1358394108-ethyl-2-methyl-4-H-pyrazolo[1,5-a]pyrazolo[4',3':5,6]pyrido[3,4-e]pyrimidin-5(8H)-one

생성물 1

HCID 227574542,4-dimethyl-8-ethyl-4H-pyrazolo[1,5-a]pyrazolo[4', 3': 5,6]pyrido[3,4-e]pyrimidin-5(8H)-one

시약·촉매·용매 1

HCID 8150Diglyme용매

실험 절차

2.7 g. of 8-ethyl-2-methyl-4-H-pyrazolo[1,5-a]pyrazolo[4',3':5,6]pyrido[3,4-e]pyrimidin-5(8H)-one (0.01 mol.) are added to a suspension of 0.03 g. of sodium hydride in 50 ml. of diethylene glycol dimethyl ether at reflux temperature. The temperature is maintained for one hour and then lowered to 120°. 2.8 g. of methyl iodide are added and heating is continued for 10 hours. The precipitated sodium iodide is filtered off, the solution evaporated to dryness and the residue recrystallized from ethyl-acetate, yield 1.9 g. (68%); m.p. 206°-207°.

후처리

  1. temperatureThe temperature is maintained for one hour
  2. customlowered to 120°
  3. temperatureheating
  4. filtrationThe precipitated sodium iodide is filtered off
  5. customthe solution evaporated to dryness
  6. customthe residue recrystallized from ethyl-acetate, yield 1.9 g

출처 및 근거

ORD 기록
ord-a06a149450b54420a041839e84b3271f
출처 데이터셋
uspto-grants-1978_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04127657

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