반응 #1781332

반응 방정식

triethylamine

4-benzyloxy-phenyl-acetohydroximoyl chloride

tetrahydrofuran

5-ethynyl-6-methyl-pyridin-2-ylamine

→

title compound

수율 58.9%

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

수율 58.9%

용매

water

반응 조건

후처리

1. 1
   기타was allowed to room temperature
2. 2
   추출the mixture was extracted with ethyl acetate
3. 3
   세척The organic layer was washed with saturated aqueous sodium chloride
4. 4
   농축was concentrated under a reduced pressure
5. 5
   기타The residue thus obtained
6. 6
   기타was purified by NH silica gel column chromatography (heptane:ethyl acetate=1:2)

실험 절차

To a mixture of 4-benzyloxy-phenyl-acetohydroximoyl chloride (59 mg, 0.21 mmol) described in Manufacturing Example 1-1-3 and tetrahydrofuran (1 mL) were added 5-ethynyl-6-methyl-pyridin-2-ylamine (22 mg, 0.16 mmol) described in Manufacturing Example 187-1-2 and triethylamine (46 μL, 0.33 mmol), which was stirred for 2 hours at 50° C. The reaction mixture was allowed to room temperature, water was added at the same temperature, and the mixture was extracted with ethyl acetate. The organic layer was washed with saturated aqueous sodium chloride, and was concentrated under a reduced pressure. The residue thus obtained was purified by NH silica gel column chromatography (heptane:ethyl acetate=1:2) to obtain the title compound (35 mg, 57%).

출처