Acetic Acid → HCID 86665323, compound

Temperature

0 °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. while an inner temperature of 0° C. or lower was maintained. After the mixed solution was stirred for 10 minutes, 4-amino-1-butanol (3.1 mL) was added dropwise while an inner temperature of 0° C. or lower was maintained. After the mixture was stirred for 10 minutes, a temperature was raised to room temperature with a water bath. After the mixture was stirred for 10 minutes, diethyl ether (100 mL) was added, and this was concentrated under reduced pressure. To the resulting concentrated material was added diethyl ether (100 mL), the mixture was stirred, and the supernatant was removed. The resulting residue was concentrated under reduced pressure to obtain a titled compound (6.31 g) having the following physical property values.

1. temperaturelower was maintained
2. temperaturelower was maintained
3. stirringAfter the mixture was stirred for 10 minutes
4. temperaturea temperature was raised to room temperature with a water bath
5. stirringAfter the mixture was stirred for 10 minutes
6. concentrationthis was concentrated under reduced pressure
7. additionTo the resulting concentrated material was added diethyl ether (100 mL)
8. stirringthe mixture was stirred
9. customthe supernatant was removed
10. concentrationThe resulting residue was concentrated under reduced pressure

ORD record

ord-a50a5ca2c3be495482a66ad7a1dd8a78

Source dataset

uspto-grants-2013_12

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US08614340B2