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Water → HCID 53446371, 화합물

HRID 2213038
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HRID 2213038 반응식
C[Si](C)(C)[N-][Si](C)(C)C.[Li+].[N:11]1([C:27]([O:29][C:30]([CH3:33])([CH3:32])[CH3:31])=[O:28])[CH2:16][CH2:15][CH:14]([C:17]([O:19][CH2:20][C:21]2[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=2)=[O:18])[CH2:13][CH2:12]1.Br[CH2:35][CH2:36][CH:37]=[CH2:38].O>O1CCCC1>[CH2:38]([C:14]1([C:17]([O:19][CH2:20][C:21]2[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=2)=[O:18])[CH2:13][CH2:12][N:11]([C:27]([O:29][C:30]([CH3:33])([CH3:32])[CH3:31])=[O:28])[CH2:16][CH2:15]1)[CH2:37][CH:36]=[CH2:35]
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참가 물질

6

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HCID 962WaterHCID 21241Homoallyl bromideHCID 2733832Lithium hexamethyldisilazaneHCID 222559134-Benzyl 1-tert-butyl piperidine-1,4-dicarboxylate

생성물 1

HCID 53446371HCID 53446371, 화합물수율 37%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran
용매

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온도
-78 °C

실험 절차

Lithium hexamethyldisilazide (1M in tetrahydrofuran, 15.7 mL, 15.7 mmol) was added dropwise to a stirred, cooled (−78° C.) solution of 1-(1,1-dimethylethyl) 4-phenylmethyl 1,4-piperidinedicarboxylate (2.50 g, 7.83 mmol) in tetrahydrofuran (50 mL) and the mixture was stirred at −78° C. for 2 hours. 4-Bromo-1-butene (1.99 mL, 19.6 mmol) was added dropwise and the mixture was stirred at −78° C. for 1 hour, then at room temperature for 2 hours. Water (100 mL) was added and the mixture was extracted with ethyl acetate (2×100 mL). The combined organic fractions were dried (MgSO4) and the solvent was evaporated under reduced pressure. The residue was purified by flash column chromatography on silica gel, eluting with isohexane/EtOAc (90:10) to give the title compound (1.07 g, 37%). 1H NMR (400 MHz CDCl3) δ 7.4–7.3 (5H, m), 5.75–5.6 (1H, m), 5.15 (2H, s), 4.93 (1H, br d, J 7 Hz), 4.90 (1H, br s), 3.95–3.75 (2H, m), 2.93–2.78 (2H, m), 2.13 (2H, br d, J 10 Hz), 1.95–1.85 (2H, m), 1.65–1.55 (2H, m), 1.44 (9H, s), and 1.43–1.30 (2H, m).

후처리

  1. stirringthe mixture was stirred at −78° C. for 1 hour
  2. waitat room temperature for 2 hours
  3. extractionthe mixture was extracted with ethyl acetate (2×100 mL)
  4. dry with materialThe combined organic fractions were dried (MgSO4)
  5. customthe solvent was evaporated under reduced pressure
  6. customThe residue was purified by flash column chromatography on silica gel
  7. washeluting with isohexane/EtOAc (90:10)

출처 및 근거

ORD 기록
ord-8cf16cbefa77473bae626586e5ed824c
출처 데이터셋
uspto-grants-2006_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07105507B2

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