Methanol → Methyl 3-amino-2-fluoropropanoate hydrochloride
반응식
S(Cl)([Cl:3])=O.[NH2:5][CH2:6][CH:7]([F:11])[C:8]([OH:10])=[O:9].[CH3:12]O>>[ClH:3].[CH3:12][O:9][C:8](=[O:10])[CH:7]([F:11])[CH2:6][NH2:5]참가 물질
4
실험 절차
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.
후처리
- temperaturemaintaining the temperature below 5° C
- customwas obtained
- customThe ice bath was removed
- stirringstirring
- concentrationThe solution was concentrated in vacuo and further co-evaporated three times with dry methanol
- filtrationThe residue was filtered off
- washwashed with DCM
- customdried
출처 및 근거
- ORD 기록
- ord-bea809f4d86040359686397c72b8a9a4
- 출처 데이터셋
- uspto-grants-2005_10
- 특허 번호
- US06953812B2
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