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Methyl iodide → 3-ethyl-3,11-dihydro-9,11-dimethyl-6H-pyrazolo[1,5-a]pyrazolo[4',3':5,6]pyrido[4,3-d]-pyrimidin-6-one

HRID 460756
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HRID 460756 반응식
[CH2:1]([N:3]1[C:7]2[N:8]=[CH:9][C:10]3[C:15](=[O:16])[N:14]4[N:17]=[C:18]([CH3:20])[CH:19]=[C:13]4[NH:12][C:11]=3[C:6]=2[CH:5]=[N:4]1)[CH3:2].[Na].[CH3:22]I>COCCOCCOC>[CH2:1]([N:3]1[C:7]2[N:8]=[CH:9][C:10]3[C:15](=[O:16])[N:14]4[N:17]=[C:18]([CH3:20])[CH:19]=[C:13]4[N:12]([CH3:22])[C:11]=3[C:6]=2[CH:5]=[N:4]1)[CH3:2]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 6328Methyl iodideHCID 5360545SodiumHCID 178462995HCID 178462995, 화합물

생성물 1

HCID 213945243-ethyl-3,11-dihydro-9,11-dimethyl-6H-pyrazolo[1,5-a]pyrazolo[4',3':5,6]pyrido[4,3-d]-pyrimidin-6-one

시약·촉매·용매 1

HCID 8150Diglyme용매

실험 절차

8.05 g. of 3-ethyl-3,11-dihydro-9-methyl-6H-pyrazolo[1,5-a]pyrazolo[4',3':5,6]pyrido[4,3-d]pyrimidin-6-one (0.03 mol.) are refluxed with stirring in 100 ml. of diethyleneglycol dimethylether together with 0.9 g. of sodium (0.04 mol.) for 2 hours. After this time, 14.2 g. of methyl iodide (0.1 mol.) are added and heating is continued for 12 hours. The solvent is removed in vacuo and the residue crystallized with methanol, filtered and washed with water to obtain 3-ethyl-3,11-dihydro-9,11-dimethyl-6H-pyrazolo[1,5-a]pyrazolo[4',3':5,6]pyrido[4,3-d]-pyrimidin-6-one, yield 5.2 g. (61%), m.p. 306°-307° (methanol).

후처리

  1. temperatureheating
  2. customThe solvent is removed in vacuo
  3. customthe residue crystallized with methanol
  4. filtrationfiltered
  5. washwashed with water

출처 및 근거

ORD 기록
ord-dfcc5fd51c4d4283b5d4c84188960425
출처 데이터셋
uspto-grants-1977_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04061632

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