Potassium Carbonate → HCID 86700048, 화합물

HRID 1428098노트

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HRID 1428098 반응식
[Br:1][C:2]1[C:3]([NH2:9])=[N:4][CH:5]=[C:6](I)[CH:7]=1.[CH3:10][O:11][C:12]1[CH:13]=[C:14](B(O)O)[CH:15]=[CH:16][C:17]=1[O:18][CH3:19].C(=O)([O-])[O-].[K+].[K+].[Cl-].[NH4+]>O1CCOCC1.O.C1C=CC([P]([Pd]([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)[P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)=CC=1>[Br:1][C:2]1[C:3]([NH2:9])=[N:4][CH:5]=[C:6]([C:15]2[CH:14]=[CH:13][C:12]([O:11][CH3:10])=[C:17]([O:18][CH3:19])[CH:16]=2)[CH:7]=1

참가 물질

8

반응물 4

HCID 11430Potassium CarbonateHCID 25517Ammonium ChlorideHCID 27347023,4-Dimethoxyphenylboronic acidHCID 176094413-Bromo-5-iodopyridin-2-amine

생성물 1

HCID 86700048HCID 86700048, 화합물수율 94.9%

시약·촉매·용매 3

HCID 178418397HCID 178418397, 화합물촉매HCID 962Water용매HCID 312751,4-Dioxane용매

실험 절차

3-Bromo-5-iodopyridin-2-amine (7.50 g), 3,4-dimethoxyphenylboronic acid (4.79 g), tetrakis(triphenylphosphine)palladium (1.45 g) and potassium carbonate (10.4 g) were suspended in dioxane (100 ml) and water (10 ml), and the suspension was heated at 80° C. for 9.5 hours. After leaving to cool, a saturated aqueous ammonium chloride solution was added, and the organic layer was extracted with ethyl acetate and dried over sodium sulfate. The solvent was distilled off under reduced pressure, and the residue was purified by silica gel column chromatography [ethyl acetate] to give 7.36 g of the title compound as a solid.

후처리

  1. customAfter leaving
  2. temperatureto cool
  3. extractionthe organic layer was extracted with ethyl acetate
  4. dry with materialdried over sodium sulfate
  5. distillationThe solvent was distilled off under reduced pressure
  6. customthe residue was purified by silica gel column chromatography [ethyl acetate]

출처 및 근거

ORD 기록
ord-a53daad04b8b4a6090092417a66ae3e6
출처 데이터셋
uspto-grants-2015_01
특허 번호
US08933103B2

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