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Toluene → Diethyl {[1-(tert-butoxycarbonyl)piperidin-4-yl]methyl}propanedioate

HRID 1386712
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HRID 1386712 반응식
[C:1]([O:5][C:6]([N:8]1[CH2:13][CH2:12][CH2:11][CH2:10][CH:9]1CI)=[O:7])([CH3:4])([CH3:3])[CH3:2].[CH2:16]1OCCOCCOCCOCCOCCO[CH2:17]1.C(=O)([O-])[O-].[K+].[K+].C([C:42]([CH2:49]C)([C:46]([O-:48])=[O:47])[C:43]([O-:45])=[O:44])C.[C:51]1(C)C=CC=C[CH:52]=1>>[C:1]([O:5][C:6]([N:8]1[CH2:9][CH2:10][CH:11]([CH2:49][CH:42]([C:46]([O:48][CH2:51][CH3:52])=[O:47])[C:43]([O:45][CH2:16][CH3:17])=[O:44])[CH2:12][CH2:13]1)=[O:7])([CH3:2])([CH3:3])[CH3:4]
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참가 물질

6

반응물 5

HCID 1140TolueneHCID 11430Potassium CarbonateHCID 2855718-Crown-6HCID 69515632,2-DiethylpropanedioateHCID 21180810tert-Butyl 2-(iodomethyl)piperidine-1-carboxylate

생성물 1

HCID 21180611Diethyl {[1-(tert-butoxycarbonyl)piperidin-4-yl]methyl}propanedioate수율 89%

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온도
80 °C

실험 절차

A mixture of 645 mg (2.0 mmol) of 1-(t-butoxycarbonyl)-4-(iodomethyl)piperidine (from EXAMPLE 32, Step A), 660 mg (2.5 mmol) of 18-crown-6, 550 mg (4.0 mmol) of potassium carbonate and 0.60 mL of diethylmalonate in 12 mL of toluene was heated at 80° C. for 20h. The mixture was cooled, partitioned between 75 mL of ether and 50 mL of H2O and the layers were separated. The organic layer was washed with 50 mL of 5% Na2S2O3, 50 mL of sat'd NaCl, dried over MgSO4 and concentrated. Flash chromatography on 30 g of silica gel using 4:1 v/v hexanes/EtOAc, then 2:1 v/v hexanes/EtOAc as the eluant afforded 630 mg (89%) of the title compound: 1H NMR (500 MHz) δ 1.07-1.14 (m, 21), 1.24-1.28 (m, 6H), 1.38-1.45 (m, 1H), 1.45 (s, 9H), 1.66 (d, J=13.0, 2H), 1.83-1.87 (m, 2H), 2.65 (t, J=7.5,22H), 3.41-3.45 (m, 1H), 4.07 (app d, J=12.5,22H), 4.194.22 (m, 2H).

후처리

  1. temperatureThe mixture was cooled
  2. custompartitioned between 75 mL of ether and 50 mL of H2O
  3. customthe layers were separated
  4. washThe organic layer was washed with 50 mL of 5% Na2S2O3, 50 mL of sat'd NaCl
  5. dry with materialdried over MgSO4
  6. concentrationconcentrated

출처 및 근거

ORD 기록
ord-24bff58b7f434bc1b488c3377fd54396
출처 데이터셋
uspto-grants-2001_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06265434B1

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