Potassium Iodide → tert-Butyl 1-(2-methoxyethyl)piperidin-4-ylcarbamate

HRID 2241405노트

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HRID 2241405 반응식
[NH:1]1[CH2:6][CH2:5][CH:4]([NH:7][C:8](=[O:14])[O:9][C:10]([CH3:13])([CH3:12])[CH3:11])[CH2:3][CH2:2]1.Br[CH2:16][CH2:17][O:18][CH3:19].[I-].[K+].C([O-])([O-])=O.[K+].[K+]>CCOC(C)=O.O.CC#N>[CH3:19][O:18][CH2:17][CH2:16][N:1]1[CH2:2][CH2:3][CH:4]([NH:7][C:8](=[O:14])[O:9][C:10]([CH3:11])([CH3:13])[CH3:12])[CH2:5][CH2:6]1

참가 물질

8

반응물 4

HCID 4875Potassium IodideHCID 11430Potassium CarbonateHCID 809722-Bromoethyl methyl etherHCID 7238334-(N-Boc-amino)piperidine

생성물 1

HCID 53256198tert-Butyl 1-(2-methoxyethyl)piperidin-4-ylcarbamate수율 77.4%

시약·촉매·용매 3

HCID 962Water용매HCID 6342Acetonitrile용매HCID 8857Ethyl Acetate용매

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온도
80 °C

실험 절차

A stirred mixture of tert-butyl piperidin-4-ylcarbamate (1.1 g, 5.5 mmol), 1-bromo-2-methoxyethane (0.69 g, 5.0 mmol), potassium iodide (0.83 g, 5.0 mmol), K2CO3 (0.69 g, 5.0 mmol) and CH3CN (10 mL) was heated to 80° C. in a sealed vessel for 18 hours. After cooling to ambient temperature, the mixture was diluted with EtOAc (15 mL) and water (15 mL). The phases were separated, and the organic phase washed with water, brine, dried (Na2SO4), filtered, and concentrated. The product was obtained as a waxy solid (1.0 g, 77%).

후처리

  1. temperatureAfter cooling to ambient temperature
  2. customThe phases were separated
  3. washthe organic phase washed with water, brine
  4. dry with materialdried (Na2SO4)
  5. filtrationfiltered
  6. concentrationconcentrated

출처 및 근거

ORD 기록
ord-ea326ba9d6804b999a43de72bf2aa306
출처 데이터셋
uspto-grants-2010_05
특허 번호
US07723330B2

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