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Chloroform → 2-(4-Dimethylamino-butyl)-5,6-dimethoxy-1-methyl-1H-quinazoline-4-one

HRID 557150
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HRID 557150 반응식
[CH3:1][N:2]([CH:4]([CH2:8][CH2:9][CH3:10])C(O)=O)[CH3:3].S(Cl)(Cl)=O.[CH3:15][NH:16][C:17]1[C:22]([C:23]([NH2:25])=[O:24])=[C:21]([O:26][CH3:27])[C:20]([O:28][CH3:29])=[CH:19][CH:18]=1.Cl[CH:31](Cl)Cl>>[CH3:1][N:2]([CH3:3])[CH2:4][CH2:8][CH2:9][CH2:10][C:15]1[N:16]([CH3:31])[C:17]2[C:22]([C:23](=[O:24])[N:25]=1)=[C:21]([O:26][CH3:27])[C:20]([O:28][CH3:29])=[CH:19][CH:18]=2
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참가 물질

5

반응물 4

HCID 6212ChloroformHCID 24386Thionyl ChlorideHCID 178834622-(Dimethylamino)pentanoic acidHCID 669909586-Methylamino-2,3-dimethoxybenzamide

생성물 1

HCID 669913772-(4-Dimethylamino-butyl)-5,6-dimethoxy-1-methyl-1H-quinazoline-4-one

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온도
57.5 °C

실험 절차

3.80 g (20.9 mmol) Dimethylamino-pentanoic acid were added to 25 ml thionyl chloride and stirred for 90 min. at 55-60° C. The remaining thionyl chloride was distilled in vacuum and the residue was added to a solution of 2.00 g (11.1 mmol) 6-methylamino-2,3-dimethoxybenzamide dissolved in 30 ml trichloromethane at 0° C. The mixture was boiled for 2 h and stirred overnight at room temperature. After filtration the residue was dissolved in trichloromethane and saturated sodium bicarbonate solution. The organic solution was dried over magnesium sulfate and evaporated under vacuum.

후처리

  1. distillationThe remaining thionyl chloride was distilled in vacuum
  2. waitThe mixture was boiled for 2 h
  3. stirringstirred overnight at room temperature
  4. filtrationAfter filtration the residue
  5. dissolutionwas dissolved in trichloromethane
  6. dry with materialThe organic solution was dried over magnesium sulfate
  7. customevaporated under vacuum

출처 및 근거

ORD 기록
ord-1a77a7c056f24f0d8f7fce86aedb7dfd
출처 데이터셋
uspto-grants-2011_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08058431B2

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