Water → HCID 22253670, compound

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 record

ord-d0fd2b590ecb48a0a9a63c1bcb0c5298

Source dataset

uspto-grants-2009_07

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US07557177B2