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Dimethylformamide → 2,11-dihydro-2-methyl-3H-s-triazolo[3,4-b][3]benzazepin-3-one

HRID 1414722
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HRID 1414722 반응식
[N:1]1[NH:2][C:3](=[O:15])[N:4]2[CH:10]=[CH:9][C:8]3[CH:11]=[CH:12][CH:13]=[CH:14][C:7]=3[CH2:6][C:5]=12.[CH3:16]N(C)C=O.[OH-].[Na+].CI>O>[CH3:16][N:2]1[C:3](=[O:15])[N:4]2[C:5]([CH2:6][C:7]3[CH:14]=[CH:13][CH:12]=[CH:11][C:8]=3[CH:9]=[CH:10]2)=[N:1]1
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참가 물질

6

반응물 4

HCID 6228DimethylformamideHCID 6328Methyl iodideHCID 14798Sodium HydroxideHCID 130667602,11-dihydro-3H-s-triazolo[3,4-b][3]benzazepin-3-one

생성물 1

HCID 130667612,11-dihydro-2-methyl-3H-s-triazolo[3,4-b][3]benzazepin-3-one

시약·촉매·용매 1

HCID 962Water용매

실험 절차

To a solution of 8 parts of 2,11-dihydro-3H-s-triazolo-[3,4-b][3]benzazepin-3-one in 80 volume parts of dimethylformamide is added 9 volume parts of 5N aqueous sodium hydroxide solution and then 3 volume parts of methyl iodide is added dropwise under stirring. After stirring for 1 hour, the reaction mixture is diluted with water and extracted with ethyl acetate. The ethyl acetate layer is washed with water and the solvent is distilled off. The precipitate is collected by filtration to give 2,11-dihydro-2-methyl-3H-s-triazolo[3,4-b][3]benzazepin-3-one as crystals. Recrystallization from isopropyl ether gives light-brown needles melting at 123° -124° C.

후처리

  1. stirringAfter stirring for 1 hour
  2. extractionextracted with ethyl acetate
  3. washThe ethyl acetate layer is washed with water
  4. distillationthe solvent is distilled off
  5. filtrationThe precipitate is collected by filtration

출처 및 근거

ORD 기록
ord-d48b59df7efa49cf8c9a8645b6cea471
출처 데이터셋
uspto-grants-1977_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04002638

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