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Methylamine → 4-(2-aminopyrimidin-5-yl)-2-fluoro-N-methylbenzenesulfonamide

HRID 500269
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HRID 500269 반응식
Br[C:2]1[CH:7]=[CH:6][C:5]([S:8](Cl)(=[O:10])=[O:9])=[C:4]([F:12])[CH:3]=1.CN.[CH2:15]([N:17](CC)CC)C.CC1(C)C(C)(C)OB([C:30]2[CH:31]=[N:32][C:33]([NH2:36])=[N:34][CH:35]=2)O1.C(=O)([O-])[O-].[K+].[K+]>C(Cl)Cl.O.C1(C)C=CC=CC=1.C(O)C.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.CCOCC>[NH2:36][C:33]1[N:32]=[CH:31][C:30]([C:2]2[CH:7]=[CH:6][C:5]([S:8]([NH:17][CH3:15])(=[O:10])=[O:9])=[C:4]([F:12])[CH:3]=2)=[CH:35][N:34]=1
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참가 물질

12

반응물 5

HCID 6329MethylamineHCID 8471TriethylamineHCID 11430Potassium CarbonateHCID 27363104-Bromo-2-fluorobenzene-1-sulfonyl chlorideHCID 177502122-Aminopyrimidine-5-boronic acid, pinacol ester

생성물 1

HCID 672251694-(2-aminopyrimidin-5-yl)-2-fluoro-N-methylbenzenesulfonamide수율 84.6%

시약·촉매·용매 6

HCID 178418397HCID 178418397, 화합물촉매HCID 702Ethanol용매HCID 962Water용매HCID 1140Toluene용매HCID 3283Diethyl Ether용매HCID 6344Dichloromethane용매

실험 절차

4-Bromo-2-fluorobenzenesulfonyl chloride (100 mg, 0.36 mmol) was added to a mixture of methylamine (2M in THF, 0.275 mL, 0.55 mmol) and triethylamine (0.10 mL, 0.73 mmol) in methylene chloride (2.0 mL). The reaction mixture was quenched with saturated NaHCO3 (1.0 mL) and concentrated to afford the crude intermediate in water. A mixture of the intermediate in water, 5-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)pyrimidin-2-amine (81 mg, 0.36 mmol), tetrakis(triphenylphosphine)palladium (20 mg, 0.02 mmol), potassium carbonate (150 mg, 1.1 mmol) in toluene (2.0 mL) and ethanol (1.0 mL) was heated at 110° C. for 2 h. After cooling to RT, ether was added to the mixture and the solid was filtered, washed with water and ether to afford the desired product (0.086 g, 83%). LCMS: (M+H)=282.9.

후처리

  1. customThe reaction mixture was quenched with saturated NaHCO3 (1.0 mL)
  2. concentrationconcentrated
  3. customto afford the crude intermediate in water
  4. filtrationthe solid was filtered
  5. washwashed with water and ether

출처 및 근거

ORD 기록
ord-4fadf6f84e47405cb4b56c44ff8d3ccb
출처 데이터셋
uspto-grants-2010_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07767675B2

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