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2-Chloro-3-nitropyridine → tert-Butyl (1-(3-nitropyridin-2-yl)piperidin-4-yl)carbamate

HRID 2233835
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HRID 2233835 반응식
[C:1]([O:5][C:6](=[O:14])[NH:7][CH:8]1[CH2:13][CH2:12][NH:11][CH2:10][CH2:9]1)([CH3:4])([CH3:3])[CH3:2].Cl[C:16]1[C:21]([N+:22]([O-:24])=[O:23])=[CH:20][CH:19]=[CH:18][N:17]=1>CN1C(=O)CCC1>[N+:22]([C:21]1[C:16]([N:11]2[CH2:12][CH2:13][CH:8]([NH:7][C:6](=[O:14])[O:5][C:1]([CH3:4])([CH3:2])[CH3:3])[CH2:9][CH2:10]2)=[N:17][CH:18]=[CH:19][CH:20]=1)([O-:24])=[O:23]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 796132-Chloro-3-nitropyridineHCID 7238334-(N-Boc-amino)piperidine

생성물 1

HCID 44120582tert-Butyl (1-(3-nitropyridin-2-yl)piperidin-4-yl)carbamate수율 83.8%

시약·촉매·용매 1

HCID 13387N-methyl-2-pyrrolidone용매

실험 절차

Anhydrous TEA (0.76 ml, 5.49 mmol) was added to piperidin-4-yl-carbamic acid tert-butyl ester (1 g, 5 mmol) and 2-chloro-3-nitro-pyridine (0.791 g, 5 mmol) in anhydrous NMP (3 ml). Using a Smith Microwave Synthesizer, the mixture was subjected to single-mode microwave at 150° C. for 10 minutes. The brown solution was partitioned between EtOAc and water and the organic phase was washed several times with water, dried over sodium sulphate and concentrated in vacuo to give the title compound as a yellow solid (1.35 g).

후처리

  1. customat 150° C.
  2. customfor 10 minutes
  3. customThe brown solution was partitioned between EtOAc and water
  4. washthe organic phase was washed several times with water
  5. dry with materialdried over sodium sulphate
  6. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-3fa3454866764ee1a3b191f0da1e0b2e
출처 데이터셋
uspto-grants-2010_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07709503B2

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