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HRID 501723作成日:2026年10月26日

Barium hydroxide, monohydrate → (2R,3S)-3-amino-4-(3,5-difluorophenyl)-1-(5-methyl-2-(pent-4-enyl)benzylamino)butan-2-ol

https://huagongshe.com/reaction/501723

反応式

関与物質

役割名称HCID仕込み量
反応物Barium hydroxide, monohydrateHCID 17749100—
反応物Benzyl (2s,3r)-1-(3,5-difluorophenyl)-3-hydroxy-4-(5-methyl-2-(pent-4-enyl)benzylamino)butan-2-ylcarbamate trifluoroacetate saltHCID 86622346—
溶媒WaterHCID 962—
溶媒1,2-DimethoxyethaneHCID 8071—
生成物(2R,3S)-3-amino-4-(3,5-difluorophenyl)-1-(5-methyl-2-(pent-4-enyl)benzylamino)butan-2-olHCID 5942382055.5%

反応条件

温度110 °C

反応手順

Step AL (2): To a solution of benzyl (2S,3R)-1-(3,5-difluorophenyl)-3-hydroxy-4-(5-methyl-2-(pent-4-enyl)benzylamino)butan-2-ylcarbamate trifluoroacetate salt (65 mg, 0.102 mmol) in DME (7.0 mL) and water (4.5 mL) was added barium hydroxide monohydrate (625 mg, 3.3 mmol). The reaction mixture was stirred at 110° C. in a high pressure vial for 18 h. The reaction mixture was filtered through a pad of celite and the filtrate was concentrated in vacuum. The residue was purified by reverse phase chromatography to give (2R,3S)-3-amino-4-(3,5-difluorophenyl)-1-(5-methyl-2-(pent-4-enyl)benzylamino)butan-2-ol double trifluoroacetate salt (22 mg, 35%) as a colorless oil. LC-MS (M+H)+=389.63.

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US07772221B2
出典データセットuspto-grants-2010_08
ORD IDord-d177d3aa82f44c129f1fc318cfe66f6d
出典メモuspto-grants-2010_08