Ethyl Acetate → 7-(4-fluorophenyl)-2-{(E)-2-[3-methoxy-4-(4-methyl-1H-imidazol-1-yl)phenyl]vinyl}-6,7-dihydro-5H-pyrrolo[1,2-b][1,2,4]triazol-7-ol

HRID 599595노트

반응식

HRID 599595 반응식
O.[Na].Cl[CH2:4][CH2:5][CH:6]([C:14]1[NH:18][C:17](/[CH:19]=[CH:20]/[C:21]2[CH:26]=[CH:25][C:24]([N:27]3[CH:31]=[C:30]([CH3:32])[N:29]=[CH:28]3)=[C:23]([O:33][CH3:34])[CH:22]=2)=[N:16][N:15]=1)[C:7]1[CH:12]=[CH:11][C:10]([F:13])=[CH:9][CH:8]=1.C(OCC)(=[O:37])C.O.C(=O)(O)[O-].[Na+]>CN(C=O)C>[F:13][C:10]1[CH:9]=[CH:8][C:7]([C:6]2([OH:37])[C:14]3[N:15]([N:16]=[C:17](/[CH:19]=[CH:20]/[C:21]4[CH:26]=[CH:25][C:24]([N:27]5[CH:31]=[C:30]([CH3:32])[N:29]=[CH:28]5)=[C:23]([O:33][CH3:34])[CH:22]=4)[N:18]=3)[CH2:4][CH2:5]2)=[CH:12][CH:11]=1

참가 물질

6

반응물 4

HCID 8857Ethyl AcetateHCID 71353970Sodium monohydrateHCID 86585896Sodium bicarbonate waterHCID 178489920HCID 178489920, 화합물

생성물 1

HCID 248531117-(4-fluorophenyl)-2-{(E)-2-[3-methoxy-4-(4-methyl-1H-imidazol-1-yl)phenyl]vinyl}-6,7-dihydro-5H-pyrrolo[1,2-b][1,2,4]triazol-7-ol

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

Sodium hydrate (containing mineral oil at 40%, 15 mg) was added to a solution of 3-[3-chloro-1-(4-fluorophenyl)propyl]-5-{(E)-2-[3-methoxy-4-(4-methyl-1H-imidazol-1-yl)phenyl]vinyl}-4H-[1,2,4]triazole (86 mg) in DMF (1 mL), and the reaction solution was stirred at room temperature for 13 hours. Ethyl acetate and saturated sodium bicarbonate water were added to the reaction solution, and the organic layer was separated. The resulting organic layer was dried over anhydrous magnesium sulfate and then concentrated under reduced pressure. The residue was purified by silica gel column chromatography (elution solvent: ethyl acetate) to obtain 3 mg of the title compound. The property values of the compound are as follows.

후처리

  1. customthe organic layer was separated
  2. dry with materialThe resulting organic layer was dried over anhydrous magnesium sulfate
  3. concentrationconcentrated under reduced pressure
  4. customThe residue was purified by silica gel column chromatography (elution solvent: ethyl acetate)

출처 및 근거

ORD 기록
ord-f5c28534a6174ff3be37d542c0c7cf8e
출처 데이터셋
uspto-grants-2011_03
특허 번호
US07897632B2

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