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Dimethylformamide → 4H-Pyrimido(6,1-a)isoquinolin-4-one, 2,3,6,7-tetrahydro-9,10-dimethoxy-3-(1-methylethyl)-2-((2,4,6-trimethylphenyl)imino)-

HRID 745310
ノート
印刷プレビュー

反応式

HRID 745310 の反応式
[CH3:1][O:2][C:3]1[CH:4]=[C:5]2[C:10](=[CH:11][C:12]=1[O:13][CH3:14])[C:9]1=[CH:15][C:16]([NH:20][C:21]3[C:26]([CH3:27])=[CH:25][C:24]([CH3:28])=[CH:23][C:22]=3[CH3:29])=[N:17][C:18](=[O:19])[N:8]1[CH2:7][CH2:6]2.CN(C)C=O.[H-].[Na+].[CH:37](I)([CH3:39])[CH3:38]>CO>[CH3:1][O:2][C:3]1[CH:4]=[C:5]2[C:10](=[CH:11][C:12]=1[O:13][CH3:14])[C:9]1=[CH:15][C:16]([N:20]([CH:37]([CH3:39])[CH3:38])[C:21]3[C:26]([CH3:27])=[CH:25][C:24]([CH3:28])=[CH:23][C:22]=3[CH3:29])=[N:17][C:18](=[O:19])[N:8]1[CH2:7][CH2:6]2.[CH3:1][O:2][C:3]1[CH:4]=[C:5]2[C:10](=[CH:11][C:12]=1[O:13][CH3:14])[C:9]1=[CH:15][C:16](=[N:20][C:21]3[C:26]([CH3:27])=[CH:25][C:24]([CH3:28])=[CH:23][C:22]=3[CH3:29])[N:17]([CH:37]([CH3:39])[CH3:38])[C:18](=[O:19])[N:8]1[CH2:7][CH2:6]2
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 6228DimethylformamideHCID 6362Isopropyl iodideHCID 24758Sodium hydrideHCID 18694579,10-dimethoxy-2-(2,4,6-trimethylanilino)-6,7-dihydropyrimido[6,1-a]isoquinolin-4-one

生成物 2

HCID 30619524H-Pyrimido(6,1-a)isoquinolin-4-one, 2,3,6,7-tetrahydro-9,10-dimethoxy-3-(1-methylethyl)-2-((2,4,6-trimethylphenyl)imino)-
HCID 3068154
4H-Pyrimido(6,1-a)isoquinolin-4-one, 6,7-dihydro-9,10-dimethoxy-2-((1-methylethyl)(2,4,6-trimethylphenyl)amino)-

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

9,10-Dimethoxy-2-(2,4,6-trimethylanilino)-6,7-dihydro-4H-pyrimido(6,1-a)isoquinolin-4-one (5.85 g) and dimethylformamide (30 ml) are added to oil-free sodium hydride (1.5 g). The mixture is heated for 5 minutes to 110° C. and then cooled to room temperature. Isopropyl iodide (2.55 g) is added and the whole is heated to 110° C. for 40 hours. After cooling, methanol is added to the reaction mixture and the solvents are removed under reduced pressure. The residue is extracted with chloroform, the extract washed with water, dried over sodium sulfate and evaporated to dryness. The residue is chromatographed to give the bases (a) m.p. 182°-183° C. and (b) m.p. 178°-179° C.

後処理

  1. temperatureThe mixture is heated for 5 minutes to 110° C.
  2. temperaturethe whole is heated to 110° C. for 40 hours
  3. temperatureAfter cooling
  4. customthe solvents are removed under reduced pressure
  5. extractionThe residue is extracted with chloroform
  6. washthe extract washed with water
  7. dry with materialdried over sodium sulfate
  8. customevaporated to dryness
  9. customThe residue is chromatographed

出典と根拠

ORDレコード
ord-171aabe56e344b2a95a6b221a6749a06
出典データセット
uspto-grants-1986_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04598148

反応ノート

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このページの内容参加物実験手順後処理出典と根拠反応ノート