Acetic Acid → HCID 86665323, compound

Temperature

-8 °C

Fuming nitric acid (1.5 mL) was added dropwise to acetic acid (25 mL) which had been cooled to an inner temperature of −8° C. with keeping an inner temperature of 0° C. or lower. After stirring the mixed solution for 10 minutes, 4-amino-1-butanol (3.1 mL) was added dropwise with keeping an inner temperature of 0° C. or lower. After stirring the mixture for 10 minutes, a temperature was raised to room temperature with a water bath. After stirring the mixture for 10 minutes, diethyl ether (100 mL) was added, followed by concentration under reduced pressure. To the resulting concentrated material, diethyl ether (100 mL) was added, followed by stirring and removing the supernatant. The resulting residue was concentrated under reduced pressure to obtain a titled compound (6.31 g) having the following physical property values.

1. customan inner temperature of 0° C.
2. customan inner temperature of 0° C.
3. stirringAfter stirring the mixture for 10 minutes
4. temperaturea temperature was raised to room temperature with a water bath
5. stirringAfter stirring the mixture for 10 minutes
6. concentrationfollowed by concentration under reduced pressure
7. additionTo the resulting concentrated material, diethyl ether (100 mL) was added
8. stirringby stirring
9. customremoving the supernatant
10. concentrationThe resulting residue was concentrated under reduced pressure

ORD record

ord-7df1133fed2d407d8032c9a52421268e

Source dataset

uspto-grants-2015_05

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US09029574B2