関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Ether hydrochloride | HCID 10953452 | — |
| 反応物 | (S)-2-tert-butoxycarbonylamino-3-difluoromethoxy-propionic acid benzyl ester | HCID 90041473 | — |
| 溶媒 | Diethyl Ether | HCID 3283 | — |
| 生成物 | (S)-2-amino-3-difluoromethoxypropionic acid benzyl ester hydrochloride salt | HCID 90040140 | 69% |
反応手順
A solution of the compound of Formula XIII(a), (S)-2-tert-butoxycarbonylamino-3-difluoromethoxy-propionic acid benzyl ester (2.11 g, 5.89 mmol) in ether (10 mL) was treated with 2M HCl/ether, and stirred at 0° C. for 2 hours. The reaction mixture was concentrated to dryness and triturated with hexane/ether to give the compound of Formula V(a) (S)-2-amino-3-difluoromethoxy-propionic acid benzyl ester hydrochloride salt (1.15 g, 69%) as a white powder. 1H NMR (300 MHz, CDCl3): δ (ppm) 7.40-7.33 (m, 5H), 6.53 (broad s, 1H), 6.18 (wt, 1H), 5.25 (dd, 1H), 5.21 (dd, 2H), 4.53 (dt, 1H) 4.18 (td, 1H), 4.16-4.13 (m, 2H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US09441012B2 |
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| 出典データセット | uspto-grants-2016_09 |
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| ORD ID | ord-53d4b22b70ed40a481fbf2687825441d |
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| 出典メモ | uspto-grants-2016_09 |
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