반응 #644449

ord-9d72e1e36d4c4d1cabd7f8038642f588

반응 조건

온도
0°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    workup.STIRRINGwas stirred for two hours at room temperature
  2. 2
    기타was allowed to room temperature
  3. 3
    추출extracted
  4. 4
    기타the organic layer was separated
  5. 5
    세척washed with saturated sodium chloride water
  6. 6
    건조dried over anhydrous magnesium sulfate
  7. 7
    기타The solvent thereof was evaporated under a reduced pressure

실험 절차

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).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US08058444B2uspto-grants-2011_11