Methanol → Methyl 3-amino-2-fluoropropanoate hydrochloride

HRID 967613노트

반응식

HRID 967613 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

  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

출처 및 근거

ORD 기록
ord-bea809f4d86040359686397c72b8a9a4
출처 데이터셋
uspto-grants-2005_10
특허 번호
US06953812B2

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