反応 #8781

反応方程式

3-[3-(3-bromo-propoxy)-phenyl]-thieno[2,3-d]isoxazole

potassium carbonate

4-methylbenzylamine

acetonitrile

→

title compound

収率 80.0%

(4-methyl-benzyl)-[3-(3-thieno[2,3-d]isoxazol-3-yl-phenoxy)-propyl]-amine

収率 80.0%

溶媒

dichloromethane

ethyl acetate

ethyl acetate

反応条件

後処理

1. 1
   温度Cool the reaction mixture
2. 2
   ろ過filter through a Waters Sep-Pak 1 g silica cartridge (ethyl acetate)
3. 3
   濃縮Combine the appropriate fractions and concentrate
4. 4
   その他to give a residue

実験手順

Mix 3-[3-(3-bromo-propoxy)-phenyl]-thieno[2,3-d]isoxazole (0.400 g, 1.18 mmol), potassium carbonate (0.326 g, 2.36 mmol), 4-methylbenzylamine (0.606, 5.00 mmol) and acetonitrile (5.0 mL) and heat (75° C.), overnight. Cool the reaction mixture and filter through a Waters Sep-Pak 1 g silica cartridge (ethyl acetate). Combine the appropriate fractions and concentrate to give a residue. Dissolved residue in 50% ethyl acetate in dichloromethane and chromatograph on silica (10 g) using ethyl acetate to give the title compound (356 mg, 80% yield). Purity by LC/MS (APCI)=98, [M+H]+=379.

出典