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

HRID 1386712
ノート
印刷プレビュー

反応式

HRID 1386712 の反応式
[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]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

6

反応物 5

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

生成物 1

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

反応条件

温度
80 °C

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-24bff58b7f434bc1b488c3377fd54396
出典データセット
uspto-grants-2001_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06265434B1

反応ノート

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