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Cesium carbonate → 6-(1,1-dimethylethyl)-5-(2-methyl-2H-1,2,4-triazol-3-ylmethoxy)-3-phenyl-1,2,3-triazolo[4,5-b]pyridine

HRID 1017637
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HRID 1017637 반응식
[C:1]1([N:7]2[C:11]3[NH:12][C:13](=[O:20])[C:14]([C:16]([CH3:19])([CH3:18])[CH3:17])=[CH:15][C:10]=3[N:9]=[N:8]2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.Cl.[CH3:22][N:23]1[C:27]([CH2:28]Cl)=[N:26][CH:25]=[N:24]1.C(=O)([O-])[O-].[Cs+].[Cs+]>CN(C=O)C.O.C(O)(=O)CC(CC(O)=O)(C(O)=O)O>[CH3:18][C:16]([C:14]1[CH:15]=[C:10]2[N:9]=[N:8][N:7]([C:1]3[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=3)[C:11]2=[N:12][C:13]=1[O:20][CH2:28][C:27]1[N:23]([CH3:22])[N:24]=[CH:25][N:26]=1)([CH3:17])[CH3:19]
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참가 물질

7

반응물 3

HCID 10796Cesium carbonateHCID 222853325-(chloromethyl)-1-methyl-1H-1,2,4-triazole hydrochlorideHCID 1358341243-Phenyl-6-(tert-butyl)-3,4-dihydro-1,2,3-triazolo[4,5-b]pyridin-5-one

생성물 1

HCID 98204146-(1,1-dimethylethyl)-5-(2-methyl-2H-1,2,4-triazol-3-ylmethoxy)-3-phenyl-1,2,3-triazolo[4,5-b]pyridine수율 83%

시약·촉매·용매 3

HCID 311
Citric Acid
용매
HCID 962Water용매
HCID 6228Dimethylformamide용매

실험 절차

A mixture of 3-phenyl-6-(tert-butyl)-3,4-dihydro-1,2,3-triazolo[4,5-b]pyridin-5-one (0.025 g, 0.093 g), 2-methyl-3-chloromethyl-1,2,4-triazole hydrochloride (0.15 g, 1.1 mmol) and cesium carbonate (0.65 g, 2.0 mmol) in dry DMF (4 ml) was stirred at r.t. for 20 h. The mixture was diluted with water (50 ml) and 1M citric acid (5 ml), and extracted with dichloromethane (2×25 ml). The extracts were dried (Na2SO4), filtered and concentrated. Preparative thin-layer chromatography, eluting with 5% methanol-dichloromethane, gave 6-(1,1-dimethylethyl)-5-(2-methyl-2H-1,2,4-triazol-3-ylmethoxy)-3-phenyl-1,2,3-triazolo[4,5-b]pyridine (0.028 g, 83%) as a white solid, m.p. 165-167° C. δH (360 MHz; CDCl3) 1.43 (9H, s), 3.94 (3H, s), 5.69 (2H, s), 7.46 (1H, t, J=7), 7.60 (2H, dd, J=7 and 7), 7.93 (1H, s), 8.20 (2H, d, J=7) and 8.31 (1H, s); m/z (ES+) 364 (M+H+).

후처리

  1. extractionextracted with dichloromethane (2×25 ml)
  2. dry with materialThe extracts were dried (Na2SO4)
  3. filtrationfiltered
  4. concentrationconcentrated
  5. washPreparative thin-layer chromatography, eluting with 5% methanol-dichloromethane

출처 및 근거

ORD 기록
ord-6f053d8340df402193106a5f7144975d
출처 데이터셋
uspto-grants-2002_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06479506B1

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