반응 #164980

반응 방정식

Water

(4-(pyridin-2-yloxymethyl)-phenyl)-acetohydroximoyl chloride

3-ethynyl-pyridin-2-ylamine

triethylamine

→

title compound

수율 26.4%

3-(3-(4-(Pyridin-2-yloxymethyl)-benzyl)-isoxazol-5-yl)-pyridin-2-ylamine

수율 26.4%

용매

tetrahydrofuran

반응 조건

후처리

1. 1
   추출was then extracted with ethyl acetate
2. 2
   세척The organic layer was washed with saturated aqueous sodium chloride
3. 3
   건조dried over anhydrous magnesium sulfate
4. 4
   기타the solvent was evaporated under a reduced pressure
5. 5
   기타The residue was purified by NH silica gel column chromatography (heptane:ethyl acetate=2:1)

실험 절차

To a solution of (4-(pyridin-2-yloxymethyl)-phenyl)-acetohydroximoyl chloride (510 mg, 1.84 mmol) described in Manufacturing Example 2-1-5 and 3-ethynyl-pyridin-2-ylamine (150 mg, 1.27 mmol) described in Manufacturing Example 1-2-3 in tetrahydrofuran (5 mL) was added triethylamine (708 μL, 5.08 mmol) at room temperature, which was stirred for 95 minutes at room temperature. Water was added at room temperature to the reaction solution, which was then extracted with ethyl acetate. The organic layer was washed with saturated aqueous sodium chloride, and dried over anhydrous magnesium sulfate, and the solvent was evaporated under a reduced pressure. The residue was purified by NH silica gel column chromatography (heptane:ethyl acetate=2:1) to obtain the title compound (120 mg, 26%).

출처