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Water → (S)-benzyl 3-(tert-butoxycarbonyl(ethyl)amino)piperidine-1-carboxylate

HRID 919579
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HRID 919579 반응식
[C:1]([O:5][C:6]([NH:8][C@H:9]1[CH2:14][CH2:13][CH2:12][N:11]([C:15]([O:17][CH2:18][C:19]2[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=2)=[O:16])[CH2:10]1)=[O:7])([CH3:4])([CH3:3])[CH3:2].[H-].[Na+].[CH2:27](Br)[CH3:28].O>CN(C=O)C>[C:1]([O:5][C:6]([N:8]([CH2:27][CH3:28])[C@H:9]1[CH2:14][CH2:13][CH2:12][N:11]([C:15]([O:17][CH2:18][C:19]2[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=2)=[O:16])[CH2:10]1)=[O:7])([CH3:4])([CH3:2])[CH3:3]
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참가 물질

6

반응물 4

HCID 962WaterHCID 6332Ethyl BromideHCID 24758Sodium hydrideHCID 50999241(S)-1-Cbz-3-Boc-Aminopiperidine

생성물 1

HCID 68070545(S)-benzyl 3-(tert-butoxycarbonyl(ethyl)amino)piperidine-1-carboxylate수율 55.5%

시약·촉매·용매 1

HCID 6228
Dimethylformamide
용매

실험 절차

To a solution of (S)-benzyl 3-(tert-butoxycarbonylamino)piperidine-1-carboxylate (500 mg, 1.49 mmol) in DMF (5 mL) was added NaH (60% suspension in mineral oil, 120 mg, 1.64 mmol) and the reaction mixture was stirred for 1 h. To the reaction mixture was added ethyl bromide (0.12 mL, 1.64 mmol) and the reaction mixture was stirred for 4 h. The reaction mixture was diluted with ice-cooled water and the solution was extracted with EtOAc, the EtOAc layer was dried over Na2SO4 and concentrated in vacuo to give the crude product that was purified by column chromatography (silica gel, gradient, EtOAc in hexanes) to give (300 mg, 55%) of the titled compound. 1H NMR (400 MHz, CDCl3): δ 7.36-7.30 (m, 5H), 5.18-5.12 (m, 2H), 4.18-4.13 (m, 2H), 3.68-3.62 (m, 1H), 3.22-3.17 (m, 2H), 3.01-2.85 (m, 1H), 2.68-2.59 (m, 1H), 1.89-1.81 (m, 1H), 1.78-1.73 (m, 2H), 1.55 (s, 9H), 1.54-1.48 (m, 1H), 1.08 (t, J=6.4 Hz, 3H). ES-MS: m/z [M+1]=363.

후처리

  1. stirringthe reaction mixture was stirred for 4 h
  2. additionThe reaction mixture was diluted with ice-
  3. extractionthe solution was extracted with EtOAc
  4. dry with materialthe EtOAc layer was dried over Na2SO4
  5. concentrationconcentrated in vacuo
  6. customto give the crude product that
  7. customwas purified by column chromatography (silica gel, gradient, EtOAc in hexanes)

출처 및 근거

ORD 기록
ord-39b3cf7c121b4431ac0bab30f976f8fe
출처 데이터셋
uspto-grants-2016_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09273028B2

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