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Cyclohexanone → 8-Cyclohexyl-3-(4-nitrophenyl)-8-azabicyclo[3.2.1]oct-2-ene

HRID 1520041
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HRID 1520041 반응식
C(O[BH-](OC(=O)C)OC(=O)C)(=O)C.[Na+].[N+:15]([C:18]1[CH:23]=[CH:22][C:21]([C:24]2[CH2:30][CH:29]3[NH:31][CH:26]([CH2:27][CH2:28]3)[CH:25]=2)=[CH:20][CH:19]=1)([O-:17])=[O:16].[C:32]1(=O)[CH2:37][CH2:36][CH2:35][CH2:34][CH2:33]1.C([O-])(O)=O.[Na+]>ClCCCl>[CH:32]1([N:31]2[CH:29]3[CH2:28][CH2:27][CH:26]2[CH:25]=[C:24]([C:21]2[CH:20]=[CH:19][C:18]([N+:15]([O-:17])=[O:16])=[CH:23][CH:22]=2)[CH2:30]3)[CH2:37][CH2:36][CH2:35][CH2:34][CH2:33]1
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참가 물질

6

반응물 4

HCID 7967CyclohexanoneHCID 516892Sodium BicarbonateHCID 5049666Sodium triacetoxyborohydrideHCID 97945973-(4-Nitrophenyl)-8-azabicyclo[3.2.1]oct-2-ene

생성물 1

HCID 679816248-Cyclohexyl-3-(4-nitrophenyl)-8-azabicyclo[3.2.1]oct-2-ene수율 65%

시약·촉매·용매 1

HCID 11
1,2-Dichloroethane
용매

실험 절차

Sodium triacetoxyborohydride (460 mg, 2.17 mmol, 2.0 eq.) was added to a solution of 3-(4-nitrophenyl)-8-azabicyclo[3.2.1]oct-2-ene (250 mg; 1.1 mmol; 1.0 eq.) and cyclohexanone (168 μl; 1.63 mmol; 1.5 eq.) in DCE (10.00 mL) and the reaction mixture was heated at 500 under nitrogen atmosphere. After 1 h, the reaction mixture was poured into a saturated solution of NaHCO3. Aqueous phase was extracted twice with DCM and combined organic phases were washed with brine, dried over magnesium sulfate, filtered and concentrated. The crude was purified by flash chromatography on silica (DCM:MeOH, gradient from 100:0 to 90:10) to give the title compound as a beige solid (220 mg, 65%). 1H NMR (300 MHz, DMSO-d6) δ 8.17 (d, J=8.9 Hz, 2H), 7.68 (d, J=8.9 Hz, 2H), 6.68 (d, J=5.4 Hz, 1H), 3.79-3.68 (m, 2H), 2.80-2.75 (m, 1H), 2.31 (m, 1H), 2.07-1.66 (m, 8H), 1.52 (m, 2H), 1.23-1.09 (m, 5H). HPLC (max plot) 100.0%; Rt %3.01 min. UPLC/MS: (MS+) 313.4.

후처리

  1. temperaturethe reaction mixture was heated at 500 under nitrogen atmosphere
  2. extractionAqueous phase was extracted twice with DCM
  3. washwere washed with brine
  4. dry with materialdried over magnesium sulfate
  5. filtrationfiltered
  6. concentrationconcentrated
  7. customThe crude was purified by flash chromatography on silica (DCM:MeOH, gradient from 100:0 to 90:10)

출처 및 근거

ORD 기록
ord-18af286035dc4750811e2df398e96266
출처 데이터셋
uspto-grants-2015_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09073892B2

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