反応 #42604

反応方程式

piperonylic acid

EDC

HOBT

3-Amino-4-(3,5-difluoro-phenyl)-1-(3-ethyl-benzylamino)-butan-2-ol

→

N-{(1S,2R)-1-(3,5-difluorobenzyl)-3-[(3-ethylbenzyl)amino]-2-hydroxypropyl}-1,3-benzodioxole-5-carboxamide

溶媒

DMF

DMF

反応条件

後処理

1. 1
   その他Reaction mixture
2. 2
   その他Quenched
3. 3
   その他reaction mixture with 10% sodium bicarbonate (aq.)
4. 4
   抽出then extracted with ethyl acetate
5. 5
   洗浄a wash with 10% sodium bicarbonate (aq.)
6. 6
   ろ過Dried organic layer over magnesium sulfate, filtered
7. 7
   濃縮concentrated in vacuo
8. 8
   その他yielding the product

実験手順

To a solution of piperonylic acid (0.500 g, 3.01 mmol), EDC (0.867 g, 4.52 mmol), HOBT (0.611 g, 4.52 mmol) in anhydrous DMF (10 mL) was added a solution of TEA (1.67 mL, 12.04 mmol), 3-Amino-4-(3,5-difluoro-phenyl)-1-(3-ethyl-benzylamino)-butan-2-ol (1.693 g, 3.01 mmol), and anhydrous DMF (5 mL). Reaction mixture was stirred under nitrogen overnight. Quenched reaction mixture with 10% sodium bicarbonate (aq.) then extracted with ethyl acetate. Washed organic layer with 1N HCl, followed by a wash with 10% sodium bicarbonate (aq.). Dried organic layer over magnesium sulfate, filtered, then concentrated in vacuo, yielding the product. (ES+: 483.2)

出典