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

HRID 12400

反応式

HRID 12400 の反応式
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

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

反応条件

温度
90 °C

実験手順

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).

後処理

  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)

出典と根拠

ORDレコード
ord-1f2d8b6dfd7647258a6c9672414d151f
出典データセット
uspto-grants-2010_06
特許番号
US07728005B2

関連ノート

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