反応 #644449

ord-9d72e1e36d4c4d1cabd7f8038642f588

反応条件

温度
0°CELSIUS
詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    workup.STIRRINGwas stirred for two hours at room temperature
  2. 2
    その他was allowed to room temperature
  3. 3
    抽出extracted
  4. 4
    その他the organic layer was separated
  5. 5
    洗浄washed with saturated sodium chloride water
  6. 6
    乾燥dried over anhydrous magnesium sulfate
  7. 7
    その他The solvent thereof was evaporated under a reduced pressure

実験手順

To a mixture of 4-(pyridin-2-yloxymethyl)-benzaldehyde described in Preparation Example 1-3-2 (24.8 g) and tetrahydrofuran (160 mL) was added methyl chloroacetate (10.2 mL) at −15° C, and sodium methoxide (23.7 mL, 28% methanol solution) was then added thereto at the same temperature. The reaction mixture was stirred at 0° C for one hour, and then was stirred for two hours at room temperature. The reaction mixture was added to ice water (800 mL) containing acetic acid (6 mL), and the reaction mixture was allowed to room temperature. To the reaction mixture was added ethyl acetate, and extracted, then, the organic layer was separated, washed with saturated sodium chloride water, and dried over anhydrous magnesium sulfate. The solvent thereof was evaporated under a reduced pressure to obtain the title compound (30.2 g).

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US08058444B2uspto-grants-2011_11