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Methanol → Methyl 3-amino-2-fluoropropanoate hydrochloride
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Methanol | HCID 887 | — |
| 反応物 | alpha-Fluoro-beta-alanine | HCID 13351 | — |
| 反応物 | Thionyl Chloride | HCID 24386 | — |
| 生成物 | Methyl 3-amino-2-fluoropropanoate hydrochloride | HCID 76026949 | 33% |
反応手順
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.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06953812B2 |
| 出典データセット | uspto-grants-2005_10 |
| ORD ID | ord-bea809f4d86040359686397c72b8a9a4 |
| 出典メモ | uspto-grants-2005_10 |