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Sodium Carbonate → HCID 178488938, 화합물

HRID 620823
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HRID 620823 반응식
O[N:2]1[C:6]([C:7]2[CH:8]=[N:9][CH:10]=[CH:11][CH:12]=2)=[C:5]([CH3:13])[N:4]=[C:3]1[C:14]1[CH:19]=[CH:18][C:17]([O:20][CH3:21])=[C:16]([O:22][CH3:23])[CH:15]=1.P(Cl)(Cl)Cl.C(=O)([O-])[O-].[Na+].[Na+]>C(Cl)Cl>[CH3:23][O:22][C:16]1[CH:15]=[C:14]([C:3]2[NH:2][C:6]([C:7]3[CH:8]=[N:9][CH:10]=[CH:11][CH:12]=3)=[C:5]([CH3:13])[N:4]=2)[CH:19]=[CH:18][C:17]=1[O:20][CH3:21]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 10340Sodium CarbonateHCID 24387Phosphorus trichlorideHCID 142113151-Hydroxy-2-(3,4-dimethoxyphenyl)-4-methyl-5-(3-pyridyl)imidazole

생성물 1

HCID 178488938HCID 178488938, 화합물수율 60.5%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

To a suspension of 1-hydroxy-2-(3,4-dimethoxyphenyl)-4-methyl-5-(3-pyridyl)imidazole (0.68 g) in methylene chloride (9 ml) was added phosphorus trichloride (0.76 ml) at ambient temperature. The mixture was refluxed for 1 hour, and cooled. The mixture was adjusted to pH 7.8 with aqueous sodium carbonate. The organic layer was separated, washed with brine, dried over magnesium sulfate, and evaporated. The residue was triturated with diisopropyl ether to give 2-(3,4-dimethoxyphenyl)-4-methyl-5-(3-pyridyl)imidazole (0.39 g).

후처리

  1. temperatureThe mixture was refluxed for 1 hour
  2. temperaturecooled
  3. customThe organic layer was separated
  4. washwashed with brine
  5. dry with materialdried over magnesium sulfate
  6. customevaporated
  7. customThe residue was triturated with diisopropyl ether

출처 및 근거

ORD 기록
ord-d7a7a69ca50a454ab5e38d10dcdb7a88
출처 데이터셋
uspto-grants-1989_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04822805

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