反応 #2275729

反応方程式

3-Amino-azetidine-1-carboxylic acid tert-butyl ester

(3-trifluoromethyl-benzoylamino)-acetic acid

EDCI

HOBT

→

title compound

3-[2-(3-Trifluoromethyl-benzoylamino)-acetylamino]azetidine-1-carboxylic acid tert-butyl ester

溶媒

DCM

反応条件

後処理

1. 1
   その他The reaction solution was partitioned between DCM and water
2. 2
   洗浄The organic layer was washed with brine
3. 3
   乾燥dried over anhydrous Na2SO4
4. 4
   ろ過filtered
5. 5
   濃縮concentrated
6. 6
   その他to give a yellow oil
7. 7
   その他purified by silica gel column on a CombiFlash® system

実験手順

3-Amino-azetidine-1-carboxylic acid tert-butyl ester (AstaTech, 1.2 g, 6.97 mmol) and (3-trifluoromethyl-benzoylamino)-acetic acid (Bionet Building Blocks, 1.57 g, 6.36 mmol) were treated with EDCI (Aldrich, 1.57 g, 6.36 mmol), HOBT (Aldrich, 1.22 g, 6.36 mmol) in DCM (10 mL) at room temperature for 4 hours. The reaction solution was partitioned between DCM and water. The organic layer was washed with brine, dried over anhydrous Na2SO4, filtered and concentrated to give a yellow oil, and purified by silica gel column on a CombiFlash® system using hexanes and ethyl acetate (from 10% ethyl acetate to 100% ethyl acetate) to afford the title compound as a white solid.

出典