Water → HCID 22253670, Verbindung

Temperatur

-12 °C

To a stirring mixture of 2-aminoisobutyric acid (52.08 g, 0.51 mol), sodium hydroxide (20.20 g, 0.51 mol), 200 mL water, and 50 mL chloroform cooled to −12° C., was added a solution of 2-bromopropionyl bromide (100 g, 0.46 mol) in 150 mL chloroform over 15 minutes. The temperature was maintained between −15 and −12° C. during the addition. The reaction mixture was then allowed to warm to room temperature and the precipitated solid was filtered. The solid was mixed with 700 mL hot toluene, and then cooled. The white solid was then filtered and dried under vacuum. A yield of 77.60 g (70%) was obtained.

1. temperatureThe temperature was maintained between −15 and −12° C. during the addition
2. temperatureto warm to room temperature
3. filtrationthe precipitated solid was filtered
4. additionThe solid was mixed with 700 mL hot toluene
5. temperaturecooled
6. filtrationThe white solid was then filtered
7. customdried under vacuum
8. customA yield of 77.60 g (70%) was obtained

ORD-Eintrag

ord-65929cf8ae0640f0aaa83641c2cb9974

Quelldatensatz

uspto-grants-2005_11

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US06969749B2