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Tetrahydrofuran → 2-chloro-4-(1-(tetrahydro-2H-pyran-2-yl)-1H-pyrazol-5-yl)benzonitrile

HRID 1409400
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HRID 1409400 반응식
Br[C:2]1[CH:9]=[CH:8][C:5]([C:6]#[N:7])=[C:4]([Cl:10])[CH:3]=1.C1COCC1.C([O-])([O-])=O.[Na+].[Na+].[O:22]1[CH2:27][CH2:26][CH2:25][CH2:24][CH:23]1[N:28]1[C:32](B2OC(C)(C)C(C)(C)O2)=[CH:31][CH:30]=[N:29]1>[Br-].C([N+](CCCC)(CCCC)CCCC)CCC.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.O.C1(C)C=CC=CC=1>[Cl:10][C:4]1[CH:3]=[C:2]([C:32]2[N:28]([CH:23]3[CH2:24][CH2:25][CH2:26][CH2:27][O:22]3)[N:29]=[CH:30][CH:31]=2)[CH:9]=[CH:8][C:5]=1[C:6]#[N:7]
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참가 물질

9

반응물 4

HCID 8028TetrahydrofuranHCID 10340Sodium CarbonateHCID 70104204-Bromo-2-chlorobenzonitrileHCID 115872081-(tetrahydro-2H-pyran-2-yl)-5-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)-1H-pyrazole

생성물 1

HCID 706562532-chloro-4-(1-(tetrahydro-2H-pyran-2-yl)-1H-pyrazol-5-yl)benzonitrile수율 91%

시약·촉매·용매 4

HCID 74236
Tetrabutylammonium Bromide
촉매
HCID 178418476HCID 178418476, 화합물촉매
HCID 962Water용매2회
HCID 1140Toluene용매

반응 조건

온도
42 °C

실험 절차

4-Bromo-2-chlorobenzonitrile (30 g, 139 mmol), 90 ml of THF and 360 ml of toluene were placed in reaction vessel under nitrogen atmosphere. Bis(triphenylphosphine)-palladium(II) chloride (4.57 g, 6.51 mmol), Na2CO3 (33.1 g, 312 mmol), 180 ml of water and tetrabutylammonium bromide (0.894 g, 2.77 mmol) were added. The reaction mixture was heated up to 42° C. 1-(Tetrahydro-2H-pyran-2-yl)-1H-pyrazole-5-boronic acid pinacol ester (42.4 g; 152 mmol) was added in three portions within one hour. The reaction was agitated at 42° C. for one hour followed with addition of 180 ml of water and cool down. The reaction mixture was filtered and layers separated. Organic phase was washed with 400 ml of water. The layers were separated and the toluene phase was distilled close to dryness. 180 ml of ethanol was added to the warm residue and the mixture was cooled down to 5° C. for three hours. The precipitate was filtered and washed with cold ethanol. 36.4 g of the title compound was obtained after vacuum drying. 1H-NMR (400 MHz, DMSO-d6): δ 1.48-1.70 (m, 3H), 1.78-1.86 (m, 1H), 1.90-2.00 (m, 1H), 2.29-2.46 (m, 1H), 3.55-3.68 (m, 1H), 3.93-4.04 (m, 1H), 5.29 (dd, 1H), 6.72 (d, 1H), 7.65 (d, 1H), 7.72 (dd, 1H), 7.92 (d, 1H), 8.13 (d, 1H).

후처리

  1. temperaturecool down
  2. filtrationThe reaction mixture was filtered
  3. customlayers separated
  4. washOrganic phase was washed with 400 ml of water
  5. customThe layers were separated
  6. distillationthe toluene phase was distilled
  7. customclose to dryness
  8. addition180 ml of ethanol was added to the warm residue
  9. temperaturethe mixture was cooled down to 5° C. for three hours
  10. filtrationThe precipitate was filtered
  11. washwashed with cold ethanol

출처 및 근거

ORD 기록
ord-cb6f52f56b5249b48f517cffae7fed5e
출처 데이터셋
uspto-grants-2014_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08921378B2

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