1-Ethyl-3-(3'-dimethylaminopropyl)carbodiimide → Tert-butyl((1r)-2,2-dimethyl-1-((4-(2-methyl-4-pyridinyl)-1-piperazinyl)carbonyl)propyl)carbamate

To a solution of Boc-D-tert-leucine (0.23 g) in methylene chloride (5 ml) were added HOBt (0.20 g), WSC (0.29 g) and triethylamine (0.28 ml) under ice-cooling, and the reaction mixture was mixed at 0° C. for 15 minutes. Then, 1-(2-methyl-4-pyridinyl)piperazine (0.18 g) obtained in Example 114b) was added thereto, and further mixed at room temperature for 13 hours. The solvent was distilled off under reduced pressure, and the residue was dissolved in ethyl acetate. The reaction mixture was washed with an aqueous potassium carbonate solution and dried over anhydrous magnesium sulfate. The solvent was distilled off under reduced pressure, and then the residue was purified with basic silica gel column (ethyl acetate) to obtain the title compound as a colorless solid (0.35 g, 90%).

1. temperaturecooling
2. additionthe reaction mixture was mixed at 0° C. for 15 minutes
3. additionfurther mixed at room temperature for 13 hours
4. distillationThe solvent was distilled off under reduced pressure
5. dissolutionthe residue was dissolved in ethyl acetate
6. washThe reaction mixture was washed with an aqueous potassium carbonate solution
7. dry with materialdried over anhydrous magnesium sulfate
8. distillationThe solvent was distilled off under reduced pressure
9. customthe residue was purified with basic silica gel column (ethyl acetate)

ORDレコード

ord-9302dbfdd2574ca7aa788a245fc8a011

出典データセット

uspto-grants-2010_10

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US07820673B2