Methanol → HCID 53420628, 화합물

HRID 1013742노트

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HRID 1013742 반응식
[F:1][C@H:2]1[CH2:6][NH:5][C@H:4]([C:7]([OH:9])=[O:8])[CH2:3]1.S(Cl)([Cl:12])=O.[CH3:14]O>>[ClH:12].[F:1][CH:2]1[CH2:6][NH:5][CH:4]([C:7]([O:9][CH3:14])=[O:8])[CH2:3]1

참가 물질

4

반응물 3

HCID 887MethanolHCID 24386Thionyl ChlorideHCID 11902999(4R)-4-Fluoro-L-proline

생성물 1

HCID 53420628HCID 53420628, 화합물

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온도
0 °C

실험 절차

A round bottom flask was charged with (2S,4R)-4-fluoropyrrolidine-2-carboxylic acid (300 mg, 2254 μmol) and 22 mL MeOH. The heterogeneous mixture was cooled to 0° C. under nitrogen, and thionyl chloride (181 μl, 2479 μmol) was added dropwise. The reaction mixture was allowed to warm slowly to RT, and stirring was continued overnight at 65° C. The mixture was concentrated under high vacuum to provide methyl 4-fluoropyrrolidine-2-carboxylate hydrochloride as a mixture of the (2S,4R) and (2R,4R) diastereomers, confirmed by 1H and 13C NMR.

후처리

  1. temperatureto warm slowly to RT
  2. concentrationThe mixture was concentrated under high vacuum

출처 및 근거

ORD 기록
ord-010488eba6cf4a2d825ef6ebca761bbf
출처 데이터셋
uspto-grants-2011_07
특허 번호
US07981891B2

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