반응 #165315

반응 방정식

triethylamine

(4-(2-furan-2-yl-ethyl)phenyl)-acetohydroximoyl chloride

tetrahydrofuran

3-ethynyl-pyridin-2,6-diamine

→

title compound

수율 73.0%

3-(3-(4-(2-Furan-2-yl-ethyl)-benzyl)-isoxazol-5-yl)-pyridin-2,6-diamine

수율 73.0%

용매

ethyl acetate

Water

반응 조건

후처리

1. 1
   기타the organic layer was separated
2. 2
   세척This organic layer was washed with water and 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 (ethyl acetate

실험 절차

To a mixture of (4-(2-furan-2-yl-ethyl)phenyl)-acetohydroximoyl chloride (100 mg, 0.38 mmol) described in Manufacturing Example 80-1-7 and tetrahydrofuran (3 mL) were added 3-ethynyl-pyridin-2,6-diamine (25.3 mg, 0.19 mmol) described in Manufacturing Example 13-1-3 and triethylamine (0.1 mL, 0.76 mmol), which was stirred for 2 hours at room temperature. Water and ethyl acetate were added to the reaction mixture, and the organic layer was separated. This organic layer was washed with water and 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 (ethyl acetate: heptane=1:1 then ethyl acetate) to obtain the title compound (50 mg, 72%).

출처