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Sodium Carbonate → HCID 11751156, 화합물

HRID 2216315
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HRID 2216315 반응식
[CH3:1][C:2]1[N:7]=[C:6]([NH:8][C:9]2[C:14]([CH3:15])=[CH:13][C:12]([CH3:16])=[CH:11][C:10]=2[CH3:17])[C:5]([S:18]([C:21]2[CH:26]=[CH:25][C:24](OS(C(F)(F)F)(=O)=O)=[CH:23][CH:22]=2)(=[O:20])=[O:19])=[CH:4][N:3]=1.[N:35]1[CH:40]=[CH:39][C:38](B(O)O)=[CH:37][CH:36]=1.C([O-])([O-])=O.[Na+].[Na+].C1C=CC(P(C2C=CC=CC=2)C2C=CC=CC=2)=CC=1.C([O-])(O)=O.[Na+]>Cl[Pd](Cl)([P](C1C=CC=CC=1)(C1C=CC=CC=1)C1C=CC=CC=1)[P](C1C=CC=CC=1)(C1C=CC=CC=1)C1C=CC=CC=1.COCCOC>[CH3:1][C:2]1[N:7]=[C:6]([NH:8][C:9]2[C:14]([CH3:15])=[CH:13][C:12]([CH3:16])=[CH:11][C:10]=2[CH3:17])[C:5]([S:18]([C:21]2[CH:26]=[CH:25][C:24]([C:38]3[CH:39]=[CH:40][N:35]=[CH:36][CH:37]=3)=[CH:23][CH:22]=2)(=[O:20])=[O:19])=[CH:4][N:3]=1
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참가 물질

8

반응물 5

HCID 10340Sodium CarbonateHCID 11776TriphenylphosphineHCID 516892Sodium BicarbonateHCID 2734379(Pyridin-4-yl)boronic acidHCID 86595018HCID 86595018, 화합물

생성물 1

HCID 11751156HCID 11751156, 화합물수율 61.1%

시약·촉매·용매 2

HCID 178418476HCID 178418476, 화합물촉매HCID 80711,2-Dimethoxyethane용매

실험 절차

A mixture trifluoromethanesulfonic acid 4-[2-methyl-4-(2,4,6-trimethylphenylamino)-pyrimidine-5-sulfonyl]-phenyl ester (72 mg, 0.14 mmol), prepared by the method described in Example 22, pyridine-4-boronic acid (34 mg, 0.28 mmol), 2 M Na2CO3 (1.0 mL, 2.0 mmol) and DME (2 mL) was deoxygenated with N2 for 10 min, and then Pd(PPh3)2Cl2 (20 mg, 0.028 mmol) and PPh3 (15 mg, 0.056 mmol) were added. The mixture was heated at reflux under N2 for 2 h and then cooled to room temperature. Saturated aqueous NaHCO3 was added, and the mixture was extracted three times with EtOAc. The combined organic layers were washed with brine, dried over Na2SO4, filtered and concentrated in vacuo. The residue was purified by chromatography on silica gel (50:50 hexanes/EtOAc) to provide the desired product (38 mg, 61%) as a white solid: mp 232–234° C.; 1H NMR (500 MHz, CDCl3) δ 8.79 (s, 1H), 8.73 (d, J=4.5 Hz, 2H), 8.28 (br s, 1H), 8.13 (d, J=8.4 Hz, 2H), 7.78 (d, J=8.4 Hz, 2H), 7.48 (d, J=4.5 Hz, 2H), 6.92 (s, 2H), 2.40 (s, 3H), 2.31 (s, 3H), 2.03 (s, 6H); APCI MS m/z 445 [(M+H)+, calcd for C25H25N4O2S, 445.2].

후처리

  1. customwas deoxygenated with N2 for 10 min
  2. temperatureThe mixture was heated
  3. temperatureat reflux under N2 for 2 h
  4. extractionthe mixture was extracted three times with EtOAc
  5. washThe combined organic layers were washed with brine
  6. dry with materialdried over Na2SO4
  7. filtrationfiltered
  8. concentrationconcentrated in vacuo
  9. customThe residue was purified by chromatography on silica gel (50:50 hexanes/EtOAc)

출처 및 근거

ORD 기록
ord-6c867fed5aa542d0a37952e451fc17ab
출처 데이터셋
uspto-grants-2006_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07112585B2

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