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Potassium Phosphate, Tribasic → HCID 136368403, 화합물

HRID 2100559
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HRID 2100559 반응식
Br[C:2]1[CH:22]=[N:21][C:5]2[N:6]=[C:7]([CH2:11][CH2:12][CH2:13][CH2:14][C:15]3[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=3)[NH:8][C:9](=[O:10])[C:4]=2[CH:3]=1.[CH:23]1(B(O)O)[CH2:25][CH2:24]1.P([O-])([O-])([O-])=O.[K+].[K+].[K+].C1(P(C2CCCCC2)C2CCCCC2)CCCCC1>C1(C)C=CC=CC=1.O.C([O-])(=O)C.[Pd+2].C([O-])(=O)C.ClCCl>[CH:23]1([C:2]2[CH:22]=[N:21][C:5]3[N:6]=[C:7]([CH2:11][CH2:12][CH2:13][CH2:14][C:15]4[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=4)[NH:8][C:9](=[O:10])[C:4]=3[CH:3]=2)[CH2:25][CH2:24]1
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참가 물질

9

반응물 4

HCID 62657Potassium Phosphate, TribasicHCID 75806TricyclohexylphosphineHCID 2760897Cyclopropylboronic acidHCID 135899296HCID 135899296, 화합물

생성물 1

HCID 136368403HCID 136368403, 화합물수율 6%

시약·촉매·용매 4

HCID 167845
palladium(II) acetate
촉매
HCID 962Water용매
HCID 1140Toluene용매
HCID 6344Dichloromethane용매

실험 절차

Palladium(II) acetate (1 mg, 4.5 μmol) was added to a degassed suspension of 6-bromo-2-(4-phenyl-butyl)-3H-pyrido[2,3-d]pyrimidin-4-one (20 mg, 55 μmol; example 26), cyclopropyl boronic acid (10 mg, 110 μmol), potassium phosphate (59 mg, 275 μmol) and tricyclohexylphosphine (3 mg, 9 μmol) in toluene (360 μl) and water (24 μl) under an argon atmosphere. The reaction mixture was heated for 14 h to 100° C. and poured onto ice cold isopropyl acetate/brine 1/1. The layers were separated, the aqueous layer was extracted two times with isopropyl acetate, the combined extracts were washed with brine and dried over sodium sulfate. Removal of the solvent under reduced pressure left a yellow solid which was purified by preparative thin layer chromatography (silica gel, isopropyl acetate/heptane) to give 6-cyclopropyl-2-(4-phenyl-butyl)-3H-pyrido[2,3-d]pyrimidin-4-one (1 mg, 3.1 μmol; 6%) as yellow crystals. MS: m/e=320.2 [M+H+].

후처리

  1. temperatureThe reaction mixture was heated for 14 h to 100° C.
  2. customThe layers were separated
  3. extractionthe aqueous layer was extracted two times with isopropyl acetate
  4. washthe combined extracts were washed with brine
  5. dry with materialdried over sodium sulfate
  6. customRemoval of the solvent under reduced pressure
  7. waitleft a yellow solid which
  8. customwas purified by preparative thin layer chromatography (silica gel, isopropyl acetate/heptane)

출처 및 근거

ORD 기록
ord-6ee95202bfaa43138ac4617bc30e2f9b
출처 데이터셋
uspto-grants-2009_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07572801B2

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