반응 #165025

반응 방정식

triethylamine

(4-benzyloxy-phenyl)-acetohydroximoyl chloride

tetrahydrofuran

3-ethynyl-6-methoxymethyl-pyridin-2-ylamine

→

title compound

수율 41.4%

3-(3-(4-Benzyloxy-benzyl)-isoxazol-5-yl)-6-methoxymethyl-pyridin-2-ylamine

수율 41.4%

용매

Water

반응 조건

후처리

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

실험 절차

To a mixture of (4-benzyloxy-phenyl)-acetohydroximoyl chloride (19 mg, 0.069 mmol) described in Manufacturing Example 1-1-3 and tetrahydrofuran (1 mL) were added 3-ethynyl-6-methoxymethyl-pyridin-2-ylamine (8.6 mg, 0.053 mmol) described in Manufacturing Example 26-1-7 and triethylamine (15 μL, 0.11 mmol) at room temperature, which was stirred for 5.5 hours at room temperature. Water was added at room temperature to the reaction mixture, which was then extracted with ethyl acetate-tetrahydrofuran (3:2). The organic layer was washed with saturated aqueous sodium chloride, and the solvent was evaporated under a reduced pressure. The residue was purified by NH silica gel column chromatography (ethyl acetate:heptane=2:3) to obtain the title compound (8.8 mg, 41%).

출처