4-Fluorophenol → (2-(4-Fluorophenoxy)-ethyl)-carbamic acid tert-butyl ester

HRID 12400

반응식

HRID 12400 반응식
Br[CH2:2][CH2:3][NH:4][C:5](=[O:11])[O:6][C:7]([CH3:10])([CH3:9])[CH3:8].[F:12][C:13]1[CH:18]=[CH:17][C:16]([OH:19])=[CH:15][CH:14]=1.C(=O)([O-])[O-].[K+].[K+]>CN(C=O)C>[F:12][C:13]1[CH:18]=[CH:17][C:16]([O:19][CH2:2][CH2:3][NH:4][C:5](=[O:11])[O:6][C:7]([CH3:10])([CH3:9])[CH3:8])=[CH:15][CH:14]=1

참가 물질

5

반응물 3

HCID 97324-FluorophenolHCID 11430Potassium CarbonateHCID 4103526tert-Butyl N-(2-bromoethyl)carbamate

생성물 1

HCID 23134036(2-(4-Fluorophenoxy)-ethyl)-carbamic acid tert-butyl ester

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

반응 조건

온도
90 °C

실험 절차

To the crude product (700 mg) of t-butyl 2-bromoethylcarbamate obtained in Step 1 were added 4-fluorophenol (875 mg), potassium carbonate (1.08 g) and DMF (7 ml), and the mixture was stirred overnight at 90° C. The solvent was evaporated, and the mixture was diluted with ethyl acetate. After washing with water, the organic layer was dried over anhydrous sodium sulfate, and the solvent was evaporated. The obtained crude product was purified by silica gel chromatography (ethyl acetate-hexane) to give t-butyl 2-(4-fluorophenoxy)ethylcarbamate (390 mg).

후처리

  1. customThe solvent was evaporated
  2. additionthe mixture was diluted with ethyl acetate
  3. washAfter washing with water
  4. dry with materialthe organic layer was dried over anhydrous sodium sulfate
  5. customthe solvent was evaporated
  6. customThe obtained crude product
  7. customwas purified by silica gel chromatography (ethyl acetate-hexane)

출처 및 근거

ORD 기록
ord-1f2d8b6dfd7647258a6c9672414d151f
출처 데이터셋
uspto-grants-2010_06
특허 번호
US07728005B2

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