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Potassium Hydroxide → 4-(2,5-Dimethyl-4-nitrophenyl)-1-(4-methoxybenzyl)piperidin-2-one

HRID 1897691
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HRID 1897691 반응식
[CH3:1][C:2]1[CH:7]=[C:6]([N+:8]([O-:10])=[O:9])[C:5]([CH3:11])=[CH:4][C:3]=1B1OC(C)(C)C(C)(C)O1.[CH3:21][O:22][C:23]1[CH:36]=[CH:35][C:26]([CH2:27][N:28]2[CH2:33][CH2:32][CH:31]=[CH:30][C:29]2=[O:34])=[CH:25][CH:24]=1.[OH-].[K+]>C1CC=CCCC=C1.C1CC=CCCC=C1.[Cl-].[Cl-].[Rh].[Rh].O1CCOCC1>[CH3:1][C:2]1[CH:7]=[C:6]([N+:8]([O-:10])=[O:9])[C:5]([CH3:11])=[CH:4][C:3]=1[CH:31]1[CH2:32][CH2:33][N:28]([CH2:27][C:26]2[CH:25]=[CH:24][C:23]([O:22][CH3:21])=[CH:36][CH:35]=2)[C:29](=[O:34])[CH2:30]1
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6

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HCID 14797Potassium HydroxideHCID 145643581-(4-Methoxybenzyl)-5,6-dihydropyridin-2(1H)-oneHCID 671555522-(2,5-Dimethyl-4-nitrophenyl)-4,4,5,5-tetramethyl-1,3,2-dioxaborolane

생성물 1

HCID 671553414-(2,5-Dimethyl-4-nitrophenyl)-1-(4-methoxybenzyl)piperidin-2-one

시약·촉매·용매 2

HCID 6436379
Rhodium, di-mu-chlorobis((1,2,5,6-eta)-1,5-cyclooctadiene)di-
촉매
HCID 312751,4-Dioxane용매

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온도
100 °C

실험 절차

In a 5 mL microwave reaction tube was added 2-(2,5-dimethyl-4-nitrophenyl)-4,4,5,5-tetramethyl-1,3,2-dioxaborolane (143 mg, 0.516 mmol, prepared from 1-bromo-2,5-dimethyl-4-nitrobenzene by standard protocol), 1-(4-methoxybenzyl)-5,6-dihydropyridin-2(1H)-one (56 mg, 0.26 mmol, prepared by following a similar procedure as reported by Lerchner etc. in Chem. Eur. J. 2006, 12, 8208), chloro(1,5-cyclooctadiene)rhodium (I) dimer (13 mg, 0.026 mmol), KOH (0.13 mL 1N aqueous solution) and dioxane (1.2 mL). The tube was degassed, filled with N2 and sealed. The reaction tube was then heated to 100° C. in a microwave reactor for 10 min. After the reaction tube was opened, the mixture was treated with saturated NH4Cl aqueous solution (3 mL) and extracted with EtOAc (3×4 mL). The organic layers were combined and concentrated. The residue was purified by flash column chromatography (silica gel, gradient 0%-70% EtOAc/hexane), to provide 4-(2,5-dimethyl-4-nitrophenyl)-1-(4-methoxybenzyl)piperidin-2-one. ESMS m/z 369.2 (M+H+).

후처리

  1. customprepared
  2. customThe tube was degassed
  3. additionfilled with N2
  4. customsealed
  5. additionthe mixture was treated with saturated NH4Cl aqueous solution (3 mL)
  6. extractionextracted with EtOAc (3×4 mL)
  7. concentrationconcentrated
  8. customThe residue was purified by flash column chromatography (silica gel, gradient 0%-70% EtOAc/hexane)

출처 및 근거

ORD 기록
ord-cfc9811cd44a4b1fb100c31b886ee20c
출처 데이터셋
uspto-grants-2013_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08519129B2

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