Hydrochloric Acid → HCID 20607351、化合物
反応式
[ClH:1].C(OC([NH:9][C@H:10]1[C@@H:14]([CH2:15][F:16])[CH2:13][NH:12][CH2:11]1)=O)(C)(C)C>O>[ClH:1].[ClH:1].[NH2:9][C@H:10]1[C@@H:14]([CH2:15][F:16])[CH2:13][NH:12][CH2:11]1参加物
4
実験手順
Concentrated hydrochloric acid (1 ml) was added to 3-(S)-tert-butoxycarbonylamino-4-(S)-fluoromethylpyrrolidine (441 mg, 2.02 mmol) which was cooled in an ice bath, and the mixture was stirred for 10 minutes. The reaction solution was mixed with water (5 ml) and washed with dichloromethane (5 ml×3) and diethyl ether (5 ml×1). The aqueous layer was concentrated under a reduced pressure, and the resulting residue was purified by its recrystallization from methanol to give 288 mg (75%) of the title compound in the form of white crystals.
後処理
- temperaturewas cooled in an ice bath
- washwashed with dichloromethane (5 ml×3) and diethyl ether (5 ml×1)
- concentrationThe aqueous layer was concentrated under a reduced pressure
- customthe resulting residue was purified by its recrystallization from methanol
出典と根拠
- ORDレコード
- ord-94292d966f7749279370642b78e9310f
- 出典データセット
- uspto-grants-2003_12
- 特許番号
- US06656952B2
反応ノート
読み込み中…