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Dimethylamine → HCID 23369747, 화합물

HRID 1900791
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HRID 1900791 반응식
[OH:1][C:2]1[CH:11]=[CH:10][C:9]([CH3:12])=[C:8]2[C:3]=1[CH:4]=[CH:5][C:6](=[O:13])[NH:7]2.[CH3:14][NH:15][CH3:16].[CH2:17]=O>CN(C)C=O>[CH3:14][N:15]([CH2:17][C:11]1[C:2]([OH:1])=[C:3]2[C:8](=[C:9]([CH3:12])[CH:10]=1)[NH:7][C:6](=[O:13])[CH:5]=[CH:4]2)[CH3:16]
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참가 물질

5

반응물 3

HCID 674Dimethylamine2회HCID 712Formaldehyde2회HCID 23369598HCID 23369598, 화합물

생성물 1

HCID 23369747HCID 23369747, 화합물수율 94.9%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매2회

실험 절차

5-Hydroxy-8-methylcarbostyril (10.51 g, 60 mmol) and dimethylamine (aqueous 40% solution, 12.07 g, 66 mmol) were dissolved in N,N-dimethylformamide (30 ml). To this solution, formaldehyde (aqueous 37% solution, 5.36 g, 66 mmol) was added slowly at room temperature, and stirred. After 12 hours, dimethylamine (6 g, 33 mmol), formaldehyde (2.79 g, 33 mmol), and N,N-dimethylformamide (20 ml) were added thereto, and the mixture was stirred at room temperature for further 12 hours. After completion of the reaction, the solvent was distilled off under reduced pressure, and the resultant residue was combined with chloroform and n-hexane. Crystals were collected by filtration, and dried under reduced pressure. As a result, 13.23 g of the title compound was obtained as pale reddish gray crystals (95%).

후처리

  1. stirringthe mixture was stirred at room temperature for further 12 hours
  2. customAfter completion of the reaction
  3. distillationthe solvent was distilled off under reduced pressure
  4. filtrationCrystals were collected by filtration
  5. customdried under reduced pressure

출처 및 근거

ORD 기록
ord-c7ec74a4c0de4bb29f0e34d12f2853fe
출처 데이터셋
uspto-grants-1996_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05576324

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