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Water → Tert-butyl [2-(2-cyanoethoxy)ethyl]carbamate

HRID 410983
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HRID 410983 반응식
[C:1]([O:5][C:6](=[O:11])[NH:7][CH2:8][CH2:9][OH:10])([CH3:4])([CH3:3])[CH3:2].C(OCC)(=O)C.O.[C:19](#[N:22])[CH:20]=[CH2:21]>>[C:1]([O:5][C:6](=[O:11])[NH:7][CH2:8][CH2:9][O:10][CH2:21][CH2:20][C:19]#[N:22])([CH3:4])([CH3:2])[CH3:3]
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참가 물질

5

반응물 4

HCID 962WaterHCID 7855AcrylonitrileHCID 8857Ethyl AcetateHCID 2733206tert-butyl N-(2-hydroxyethyl)carbamate

생성물 1

HCID 85735740Tert-butyl [2-(2-cyanoethoxy)ethyl]carbamate

반응 조건

온도
50 °C

실험 절차

[2-(2-Cyano-ethoxy)-ethyl]-carbamic acid tert-butyl ester (430 mg) was prepared starting from (2-hydroxy-ethyl)-carbamic acid tert-butyl ester (320 mg) in acrylonitrile (1.5 mL). The reaction was heated to 50° C. for 1 h. The reaction was added to ethyl acetate (20 mL) and water (20 mL). The phases were separated and the aqueous phase was extracted twice with ethyl acetate. The combined organics were dried over sodium sulfate and then filtered. The solvent was evaporated and crude compound was purified by flash chromatography using hexane:ethyl actetate gradient.

후처리

  1. customThe phases were separated
  2. extractionthe aqueous phase was extracted twice with ethyl acetate
  3. dry with materialThe combined organics were dried over sodium sulfate
  4. filtrationfiltered
  5. customThe solvent was evaporated
  6. customcrude compound was purified by flash chromatography

출처 및 근거

ORD 기록
ord-a94ddfcfea13446c80c4efd454500b28
출처 데이터셋
uspto-grants-2014_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08759535B2

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