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

반응식

HRID 543546 반응식
[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]

참가 물질

6

반응물 4

HCID 24758Sodium hydrideHCID 27661876a,7,8,9-tetrahydropyrido[3,2-e]pyrrolo[1,2-a]pyrazin-6(5H)-oneHCID 127070022-(chloromethyl)-1,3-dimethoxyBenzeneHCID 178418361HCID 178418361, 화합물

생성물 1

HCID 133420805-[(2,6-dimethoxyphenyl)methyl]-6a,7,8,9-tetrahydropyrido[3,2-e]pyrrolo[1,2-a]pyrazin-6(5H)-one수율 89%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

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.

후처리

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

출처 및 근거

ORD 기록
ord-6583a93d32e343f8b31f9da4155b9909
출처 데이터셋
uspto-grants-1984_05
특허 번호
US04446323

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