Sodium hydride → 5-[(2,6-dimethoxyphenyl)methyl]-6a,7,8,9-tetrahydropyrido[3,2-e]pyrrolo[1,2-a]pyrazin-6(5H)-one

HRID 543546

反応式

HRID 543546 の反応式
[N:1]1[C:10]2[N:9]3[CH2:11][CH2:12][CH2:13][CH:8]3[C:7](=[O:14])[NH:6][C:5]=2[CH:4]=[CH:3][CH:2]=1.[H-].[Na+].[H][H].[CH3:19][O:20][C:21]1[CH:28]=[CH:27][CH:26]=[C:25]([O:29][CH3:30])[C:22]=1[CH2:23]Cl>CN(C)C=O>[CH3:30][O:29][C:25]1[CH:26]=[CH:27][CH:28]=[C:21]([O:20][CH3:19])[C:22]=1[CH2:23][N:6]1[C:5]2[CH:4]=[CH:3][CH:2]=[N:1][C:10]=2[N:9]2[CH2:11][CH2:12][CH2:13][CH:8]2[C:7]1=[O:14]

参加物

6

実験手順

To a stirred solution of 6a,7,8,9-tetrahydropyrido[3,2-e]pyrrolo[1,2-a]pyrazin-6(5H)-one (2.7 g. 0.01 mole) in 30 ml. of dry dimethyl formamide was added sodium hydride (0.5 g., 0.02 mole of 50% dispersion in mineral oil). When the evolution of hydrogen subsides, 2.7 g. (0.01 mole) of 2,6-dimethoxybenzyl chloride was added. The reaction mixture was stirred at room temperature for eighteen hours, and the dimethyl formamide was removed under vacuo. The residue was triturated with cold water, filtered and recrystallized from ethanol to give white crystals of the title compound, 2.7 g. (89% yield) m.p. 200°-202° C.; hydrochloride salt, m.p. 220°-223° C.

後処理

  1. customthe dimethyl formamide was removed under vacuo
  2. customThe residue was triturated with cold water
  3. filtrationfiltered
  4. customrecrystallized from ethanol

出典と根拠

ORDレコード
ord-6583a93d32e343f8b31f9da4155b9909
出典データセット
uspto-grants-1984_05
特許番号
US04446323

関連ノート

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