Methanol → Methyl 3-amino-2-fluoropropanoate hydrochloride

Dry methanol (5.3 mL) was cooled to −15° C. on an ice bath and thionyl chloride (2.5 mL) was added dropwise maintaining the temperature below 5° C. To this cold solution was added (RS)-3-amino-2-fluoropropionic acid (0.27 g, 2.52 mmol) and stirring was continued until a homogeneous solution was obtained. The ice bath was removed and stirring was continued for 17 hours at room temperature. The solution was concentrated in vacuo and further co-evaporated three times with dry methanol. The residue was filtered off, washed with DCM and dried to afford 0.13 g (33%) of 3-amino-2-fluoropropionic acid methyl ester hydrochloride as a solid.

1. temperaturemaintaining the temperature below 5° C
2. customwas obtained
3. customThe ice bath was removed
4. stirringstirring
5. concentrationThe solution was concentrated in vacuo and further co-evaporated three times with dry methanol
6. filtrationThe residue was filtered off
7. washwashed with DCM
8. customdried

ORDレコード

ord-f00c308120f346e488c02df4dcb90d71

出典データセット

uspto-grants-2003_05

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US06562807B2