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Cesium carbonate → HCID 53949865, 화합물

HRID 2093470
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HRID 2093470 반응식
[N:1]1([C:13]([O:15][C:16]([CH3:19])([CH3:18])[CH3:17])=[O:14])[CH2:6][CH2:5][CH:4]([CH:7]2[CH2:12][CH2:11][NH:10][CH2:9][CH2:8]2)[CH2:3][CH2:2]1.Br[C:21]1[CH:30]=[CH:29][C:24]([C:25]([O:27][CH3:28])=[O:26])=[CH:23][CH:22]=1.C(=O)([O-])[O-].[Cs+].[Cs+].CN1C(=O)CCC1>ClCCl.CC([O-])=O.CC([O-])=O.[Pd+2]>[C:16]([O:15][C:13]([N:1]1[CH2:6][CH2:5][CH:4]([CH:7]2[CH2:12][CH2:11][N:10]([C:21]3[CH:30]=[CH:29][C:24]([C:25]([O:27][CH3:28])=[O:26])=[CH:23][CH:22]=3)[CH2:9][CH2:8]2)[CH2:3][CH2:2]1)=[O:14])([CH3:19])([CH3:18])[CH3:17]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 10796Cesium carbonateHCID 12081Methyl 4-bromobenzoateHCID 13387N-methyl-2-pyrrolidoneHCID 117475994,4'-Bipiperidine, 1-boc protected

생성물 1

HCID 53949865HCID 53949865, 화합물

시약·촉매·용매 2

HCID 167845palladium(II) acetate촉매
HCID 6344
Dichloromethane
용매

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온도
90 °C

실험 절차

A 100 mL reaction flask was charged with tert-butyl 4,4′-bipiperidine-1-carboxylate (1.14 g; 4.25 mmol), methyl 4-bromobenzoate (913 mg; 4.25 mmol), cesium carbonate (4.15 g; 12.74 mmol), Pd(OAc)2 (48 mg; 0.212 mmol) and 2-(diphenylphosphino)-2′-(N—N-dimethylamino)biphenyl (162 mg; 0.425 mmol). NMP (outgassed by bubbling with nitrogen for 10 min; 10 mL) was added and the mixture stirred at 90° C. for 18 hr. The mixture was diluted with dichloromethane (100 mL) and filtered through Celite. The filtrate was washed with water (4×25 mL). The organic was dried over magnesium sulfate, filtered and evaporated to a solid. The solid was digested at reflux (MTBE). After cooling, the white solid was recovered by filtration. The filtrate was evaporated and chromatographed (Horizon; 0% to 100% EtOAc/hex; linear gradient). The fractions containing the desired compound were recovered and combined with the solid to give the title compound.

후처리

  1. customA 100 mL reaction flask
  2. filtrationfiltered through Celite
  3. washThe filtrate was washed with water (4×25 mL)
  4. dry with materialThe organic was dried over magnesium sulfate
  5. filtrationfiltered
  6. customevaporated to a solid
  7. temperatureat reflux (MTBE)
  8. temperatureAfter cooling
  9. filtrationthe white solid was recovered by filtration
  10. customThe filtrate was evaporated
  11. customchromatographed (Horizon; 0% to 100% EtOAc/hex; linear gradient)
  12. additionThe fractions containing the desired compound
  13. customwere recovered

출처 및 근거

ORD 기록
ord-9839bc850ded4e65ae5a68b56aaff673
출처 데이터셋
uspto-grants-2013_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08445499B2

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