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Benzyl Bromide → 1-(t-Butoxycarbonyl)-4-(3-phenyl-2,2-bis(carboethoxy)propyl)piperidine

HRID 1386713
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HRID 1386713 반응식
[C:1]([O:5][C:6]([N:8]1[CH2:13][CH2:12][CH:11]([CH2:14][CH:15]([C:21]([O:23][CH2:24][CH3:25])=[O:22])[C:16]([O:18][CH2:19][CH3:20])=[O:17])[CH2:10][CH2:9]1)=[O:7])([CH3:4])([CH3:3])[CH3:2].C[Si]([N-][Si](C)(C)C)(C)C.[Na+].[CH2:36](Br)[C:37]1[CH:42]=[CH:41][CH:40]=[CH:39][CH:38]=1>C1COCC1>[C:1]([O:5][C:6]([N:8]1[CH2:9][CH2:10][CH:11]([CH2:14][C:15]([C:16]([O:18][CH2:19][CH3:20])=[O:17])([C:21]([O:23][CH2:24][CH3:25])=[O:22])[CH2:36][C:37]2[CH:42]=[CH:41][CH:40]=[CH:39][CH:38]=2)[CH2:12][CH2:13]1)=[O:7])([CH3:4])([CH3:2])[CH3:3]
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참가 물질

5

반응물 3

HCID 7498Benzyl BromideHCID 2724254Sodium bis(trimethylsilyl)amideHCID 21180611Diethyl {[1-(tert-butoxycarbonyl)piperidin-4-yl]methyl}propanedioate

생성물 1

HCID 211806581-(t-Butoxycarbonyl)-4-(3-phenyl-2,2-bis(carboethoxy)propyl)piperidine수율 96.5%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

실험 절차

A solution of 628 mg (1.76 mmol) of 1-(t-butoxycarbonyl)-4-(2,2-bis(carbethoxy)ethyl)piperidine (from EXAMPLE 32, Step B) in 8 mL of THF at 0° C. was treated with 2.0 mL of 1.0 M sodium bis(trimethylsilyl) amide solution in THF and stirred cold for 10 min. The resulting mixture was treated with 0.35 mL (2.9 mmol) of benzyl bromide then warmed to rt and stirred for 1 h. The reaction was quenched with 10 mL of sat'd NH4Cl and the quenched mixture was partitioned between 50 mL of ether and 25 mL of H2O. The layers were separated and the organic layer was washed with 25 mL of sat'd NaCl, dried over MgSO4 and concentrated. Flash chromatography on 30 g of silica gel using 4:1 v/v hexanes/ether afforded 760 mg (96%) of the title compound: 1H NMR (500 MHz) δ 1.08-1.16 (m, 2H), 1.23 (t, J=7.0,66H), 1.45 (s, 9H), 1.54-1.58 (m, 2H), 1.60-1.66 (m, 1H), 1.78 (d, J=6.0, 2H), 2.68 (app t, J=11.5, 21), 3.28 (s, 2H), 4.01 (br s, 2H), 4.15 (q, J=7.0, 4H), 7.06-7.25 (5H).

후처리

  1. stirringstirred for 1 h
  2. customThe reaction was quenched with 10 mL of sat'd NH4Cl
  3. customthe quenched mixture was partitioned between 50 mL of ether and 25 mL of H2O
  4. customThe layers were separated
  5. washthe organic layer was washed with 25 mL of sat'd NaCl
  6. dry with materialdried over MgSO4
  7. concentrationconcentrated

출처 및 근거

ORD 기록
ord-e93333eda1244a4d976d54edcf3ff960
출처 데이터셋
uspto-grants-2001_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06265434B1

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