Sulfuric Acid → 2-Methoxyethyl 3-amino-3-phenylpropionate

温度

60 °C

To 6.00 mL (76.3 mmol) of 2-methoxyethanol were added 2.00 g (12.1 mmol) of 3-amino-3-phenylpropionic acid (racemic mixture) synthesized in Reference example 1 and 1.78 g (18.2 mmol) of conc. sulfuric acid, and the mixture was reacted under stirring at 60° C. for 4 hours. After completion of the reaction, the resulting reaction mixture was concentrated under reduced pressure, and then, 6 mol/L aqueous sodium hydroxide solution was added to the reaction mixture to adjust a pH thereof to 8.5. Then, 10 mL of ethyl acetate and 4 mL of water were added to the mixture to carry out extraction, and the organic layer was dried over anhydrous magnesium sulfate. After filtration, the filtrate was concentrated under reduced pressure to obtain 2.22 g (Isolation yield based on 3-amino-3-phenylpropionic acid (racemic mixture): 82.2%) of 2-methoxyethyl 3-amino-3-phenylpropionate (racemic mixture) as colorless liquid.

1. customthe mixture was reacted
2. customAfter completion of the reaction
3. customthe resulting reaction mixture
4. concentrationwas concentrated under reduced pressure
5. addition6 mol/L aqueous sodium hydroxide solution was added to the reaction mixture
6. additionThen, 10 mL of ethyl acetate and 4 mL of water were added to the mixture
7. extractionextraction
8. dry with materialthe organic layer was dried over anhydrous magnesium sulfate
9. filtrationAfter filtration
10. concentrationthe filtrate was concentrated under reduced pressure
11. customto obtain 2.22 g (Isolation yield based on 3-amino-3-phenylpropionic acid (racemic mixture): 82.2%) of 2-methoxyethyl 3-amino-3-phenylpropionate (racemic mixture) as colorless liquid

ORDレコード

ord-74ed671cabf24bd5bceb58fe5c3f67ac

出典データセット

uspto-grants-2011_03

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US07915019B2