Dimethylformamide → HCID 178421800, 화합물

HRID 25082

반응식

HRID 25082 반응식
[CH3:1][CH:2]1[CH2:8][C:7]2[CH:9]=[C:10]3[O:15][CH2:14][O:13][C:11]3=[CH:12][C:6]=2[C:5]([C:16]2[CH:21]=[CH:20][C:19]([N+:22]([O-:24])=[O:23])=[CH:18][CH:17]=2)=[N:4][N:3]1[C:25]#[N:26].CN(C)C=O.[N-:32]=[N+:33]=[N-:34].[Na+].[Cl-].[NH4+]>O>[CH3:1][CH:2]1[CH2:8][C:7]2[CH:9]=[C:10]3[O:15][CH2:14][O:13][C:11]3=[CH:12][C:6]=2[C:5]([C:16]2[CH:17]=[CH:18][C:19]([N+:22]([O-:24])=[O:23])=[CH:20][CH:21]=2)=[N:4][N:3]1[C:25]1[NH:34][N:33]=[N:32][N:26]=1

참가 물질

6

반응물 4

HCID 6228DimethylformamideHCID 25517Ammonium ChlorideHCID 33557Sodium AzideHCID 12137416(+/-)-8-Methyl-5-(4-nitrophenyl)-8,9-dihydro-7H-1,3-dioxolo[4,5-h][2,3]benzodiazepine-7-carbonitrile

생성물 1

HCID 178421800HCID 178421800, 화합물수율 101.7%

시약·촉매·용매 1

HCID 962Water용매

반응 조건

온도
140 °C

실험 절차

A mixture of 0.60 g (1.70 mmol) of the starting material XXIII, 3 ml of dimethylformamide, 0.12 g (1.87 mmol) of sodium azide and 0.10 g (1.87 mmol) of ammonium chloride was stirred at 140° C. for 30 min. The cooled reaction mixture was diluted with water and the precipitated crystals were filtered off. The so obtained product was purified by column chromatography using silica gel (MN Kieselgel 60) as adsorbent and a mixture of chloroform-methanol (99:1) as eluent to yield 0.68 g (54%) of the title compound; Mp.: 263-264° C.

후처리

  1. customThe cooled reaction mixture
  2. filtrationthe precipitated crystals were filtered off
  3. customThe so obtained product
  4. customwas purified by column chromatography
  5. additiona mixture of chloroform-methanol (99:1) as eluent

출처 및 근거

ORD 기록
ord-2ca105df26b446e984445b4e84d6a6c2
출처 데이터셋
uspto-grants-2005_02
특허 번호
US06858605B2

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