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Potassium Carbonate → HCID 67201862, 화합물

HRID 1505992
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HRID 1505992 반응식
[C:1]([O:5][C:6]([N:8]1[CH2:13][CH2:12][C:11](=[CH2:14])[CH2:10][CH2:9]1)=[O:7])([CH3:4])([CH3:3])[CH3:2].C12BC(CCC1)CCC2.[C:24]1([S:30]([N:33]2[C:37]3[CH:38]=[N:39][C:40]([C:43]#[N:44])=[C:41](Br)[C:36]=3[C:35]3[CH:45]=[CH:46][CH:47]=[N:48][C:34]2=3)(=[O:32])=[O:31])[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=1.C(=O)([O-])[O-].[K+].[K+]>O.CN(C=O)C.ClCCl.C1C=CC(P([C]2[CH][CH][CH][CH]2)C2C=CC=CC=2)=CC=1.C1C=CC(P([C]2[CH][CH][CH][CH]2)C2C=CC=CC=2)=CC=1.Cl[Pd]Cl.[Fe]>[C:1]([O:5][C:6]([N:8]1[CH2:13][CH2:12][CH:11]([CH2:14][C:41]2[C:36]3[C:35]4[CH:45]=[CH:46][CH:47]=[N:48][C:34]=4[N:33]([S:30]([C:24]4[CH:25]=[CH:26][CH:27]=[CH:28][CH:29]=4)(=[O:32])=[O:31])[C:37]=3[CH:38]=[N:39][C:40]=2[C:43]#[N:44])[CH2:10][CH2:9]1)=[O:7])([CH3:4])([CH3:3])[CH3:2]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

9

반응물 4

HCID 11430Potassium CarbonateHCID 789669-Borabicyclo(3.3.1)nonaneHCID 27568081-Boc-4-MethylenepiperidineHCID 58266792HCID 58266792, 화합물

생성물 1

HCID 67201862HCID 67201862, 화합물수율 38%

시약·촉매·용매 4

HCID 178477754
HCID 178477754, 화합물
촉매
HCID 962Water용매2회
HCID 6228Dimethylformamide용매
HCID 6344Dichloromethane용매

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온도
65 °C

실험 절차

A mixture of 4-methylene-piperidine-1-carboxylic acid tert-butyl ester (0.70 g, 3.55 mmol) and 9-borabicyclo[3,3,1]nonane (0.5M solution in THF, 7 mL, 3.5 mmol) were heated at reflux for 1.5 h. The reaction mixture was cooled and added to a degassed mixture of 9-benzenesulfonyl-5-bromo-9H-dipyrido[2,3-b;4′,3′-d]pyrrole-6-carbonitrile (0.41 g, 1.0 mmol), [1,1-bis(diphenylphosphino) ferrocene]dichloropalladium(II) (0.090 g, 0.11 mmol) and potassium carbonate (0.18 g, 1.3 mmol) in water (1 mL) and DMF (10 mL) and the reaction mixture was then heated at 65° C. for 1.25 h. After cooling to ambient temperature the reaction mixture was then diluted with water (5 mL) and dichloromethane (10 mL). The aqueous phase was extracted with dichloromethane (2×15 mL) and the combined organic phase was washed with brine (15 mL), dried over magnesium sulfate, filtered and concentrated in vacuo. The residue was triturated with pentane (10 mL) and the resultant material was purified by flash chromatography (silica, 5 g column, SPE-Si II, 0-2% methanol in DCM) to afford title compound as a yellow solid (202 mg, 38%). 1H NMR (CDCl3, 400 MHz): 9.81 (s, 1H), 8.79 (dd, J=4.8, 1.6 Hz, 1H), 8.33-8.27 (m, 3H), 7.66-7.60 (m, 1H), 7.55-7.46 (m, 3H), 4.22-4.01 (m, 2H), 3.34-3.27 (m, 2H), 2.62-2.50 (m, 2H), 1.97-1.76 (m, 2H), 1.72-1.46 (m, 3H), 1.45 (s, 9H).

후처리

  1. temperaturewere heated
  2. temperatureat reflux for 1.5 h
  3. temperatureThe reaction mixture was cooled
  4. temperatureAfter cooling to ambient temperature the reaction mixture
  5. extractionThe aqueous phase was extracted with dichloromethane (2×15 mL)
  6. washthe combined organic phase was washed with brine (15 mL)
  7. dry with materialdried over magnesium sulfate
  8. filtrationfiltered
  9. concentrationconcentrated in vacuo
  10. customThe residue was triturated with pentane (10 mL)
  11. customthe resultant material was purified by flash chromatography (silica, 5 g column, SPE-Si II, 0-2% methanol in DCM)

출처 및 근거

ORD 기록
ord-39115b69ea7744dd81d5386433d45ad1
출처 데이터셋
uspto-grants-2015_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09216980B2

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