تفاعل #165023

معادلة التفاعل

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

thioanisole

sodium hydrogen carbonate

→

title compound

المردود 95.0%

4-(5-(2,6-Diamino-pyridine-3-yl)-isoxazol-3-ylmethyl)-phenol

المردود 95.0%

المذيبات

trifluoroacetic acid

ظروف التفاعل

المعالجة

1. 1
   استخلاصwhich was then extracted with ethyl acetate
2. 2
   غسيلThe organic layer was washed with water and saturated aqueous sodium chloride
3. 3
   تجفيفdried over anhydrous magnesium sulfate
4. 4
   أخرىthe solvent was evaporated under a reduced pressure
5. 5
   أخرىThe residue was purified by silica gel column chromatography (ethyl acetate)

الإجراء التجريبي

To a solution of 3-(3-(4-benzyloxy-benzyl)-isoxazol-5-yl)-pyridin-2,6-diamine (100 mg, 0.27 mmol) described in Example 13 in trifluoroacetic acid (3 mL) was added thioanisole (126 μl) at room temperature, which was stirred for 2 hours at room temperature. Saturated aqueous sodium hydrogen carbonate solution was added to the reaction solution at 0° C., which was then extracted with ethyl acetate. The 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 silica gel column chromatography (ethyl acetate) to obtain the title compound (72.4 mg, 95%).

المصدر