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Potassium Carbonate → HCID 66656356, 화합물

HRID 1619674
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HRID 1619674 반응식
Cl[C:2]1[CH:7]=[CH:6][C:5]([OH:8])=[C:4]([C:9]2[C:10]([N+:20]([O-:22])=[O:21])=[N:11][N:12]([CH:14]3[CH2:19][CH2:18][CH2:17][CH2:16][O:15]3)[CH:13]=2)[CH:3]=1.[C:23]([C:25]1[CH:26]=[C:27](B(O)O)[CH:28]=[CH:29][CH:30]=1)#[N:24].F[B-](F)(F)F.C([PH+](C(C)(C)C)C(C)(C)C)(C)(C)C.C(=O)([O-])[O-].[K+].[K+].C([N+](CCCC)(CCCC)CCCC)CCC>C1C(/C(/C2[C-]=CC(Cl)=CC=2)=N\O)=CC=C(Cl)C=1.C1C(/C(/C2[C-]=CC(Cl)=CC=2)=N\O)=CC=C(Cl)C=1.[Cl-].[Cl-].[Pd+2].[Pd+2].CN(C=O)C>[OH:8][C:5]1[CH:6]=[CH:7][C:2]([C:29]2[CH:28]=[CH:27][CH:26]=[C:25]([C:23]#[N:24])[CH:30]=2)=[CH:3][C:4]=1[C:9]1[C:10]([N+:20]([O-:22])=[O:21])=[N:11][N:12]([CH:14]2[CH2:19][CH2:18][CH2:17][CH2:16][O:15]2)[CH:13]=1
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참가 물질

8

반응물 5

HCID 11430Potassium CarbonateHCID 16028TetrabutylammoniumHCID 27343253-Cyanophenylboronic acidHCID 2734635Tri-tert-butylphosphine tetrafluoroborateHCID 594366304-chloro-2-[3-nitro-1-(tetrahydro-2H-pyran-2-yl)-1H-pyrazol-4-yl]phenol

생성물 1

HCID 66656356HCID 66656356, 화합물
수율 42.1%

시약·촉매·용매 2

HCID 54751178Najera Catalyst I촉매HCID 6228Dimethylformamide용매

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온도
130 °C

실험 절차

4-Chloro-2-(3-nitro-1-(tetrahydro-2H-pyran-2-yl)-1H-pyrazol-4-yl)phenol (500 mg, 1.544 mmol), 3-cyanophenylboronic acid (453 mg, 3.09 mmol), di-mu-chlorobis[5-chloro-2-[(4-chlorophenyl)(hydroxyimino)methyl]phenyl]palladium (II) dimer (63 mg, 0.0772 mmol), tri-tert-butylphosphonium tetrafluoroborate (45 mg, 0.154 mmol), potassium carbonate (426 mg, 3.09 mmol) and tetrabutyl ammonium hydroxyde solution (1M in MeOH, 0.31 mL, 0.31 mmol) were combined in a microwave vial. DMF (7.5 mL) was added and the vial was sealed. The mixture was heated at 130° C. for 1 hour under microwave irradiation and then partitioned between ethyl acetate (25 mL) and water (10 mL). The organic layer was separated and washed with brine (10 mL), dried over anhydrous MgSO4, filtered and concentrated in vacuo. The residue was purified on silica gel by Biotage™ (10% to 80% EtOAc in heptane over 20 CV) to give the title compound (254 mg, 41%) as brown oil

후처리

  1. customthe vial was sealed
  2. custompartitioned between ethyl acetate (25 mL) and water (10 mL)
  3. customThe organic layer was separated
  4. washwashed with brine (10 mL)
  5. dry with materialdried over anhydrous MgSO4
  6. filtrationfiltered
  7. concentrationconcentrated in vacuo
  8. customThe residue was purified on silica gel by Biotage™ (10% to 80% EtOAc in heptane over 20 CV)

출처 및 근거

ORD 기록
ord-0b5b7a1763fd46cd95fa363278e4b60a
출처 데이터셋
uspto-grants-2014_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08772293B2

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