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HRID 352378作成日:2026年10月25日

Hexane → (R)-(-)-1-tert-butylcarbonylmethyl-2-oxo-3-amino-5-cyclohexyl-1,3,4,5-tetrahydro-2H-1,5-benzodiazepine oxalate monohydrate

https://huagongshe.com/reaction/352378

反応式

関与物質

役割名称HCID仕込み量
反応物HexaneHCID 8058—
反応物Oxalic acid dihydrateHCID 61373—
反応物(R)-1-tert-butylcarbonylmethyl-2-oxo-3-amino-5-cyclohexyl-1,3,4,5-tetrahydro-2H-1,5-benzodiazepineHCID 11190074—
溶媒Ethyl AcetateHCID 8857—
生成物(R)-(-)-1-tert-butylcarbonylmethyl-2-oxo-3-amino-5-cyclohexyl-1,3,4,5-tetrahydro-2H-1,5-benzodiazepine oxalate monohydrateHCID 69908115—

反応手順

The (R)-(−)-1-tert-butylcarbonylmethyl-2-oxo-3-amino-5-cyclohexyl-1,3,4,5-tetrahydro-2H-1,5-benzodiazepine thus obtained was dissolved in 550 ml of ethyl acetate. To the resulting solution was added 16.31 g of oxalic acid dihydrate to dissolve the latter in the former. Then, 367 ml of n-hexane was added and the mixture was stirred overnight. Crystals so precipitated were collected by filtration with suction, washed with a mixed solvent of ethyl acetate and n-hexane (1:1), and then dried, whereby 55 g of (R)-(−)-1-tert-butylcarbonylmethyl-2-oxo-3-amino-5-cyclohexyl-1,3,4,5-tetrahydro-2H-1,5-benzodiazepine oxalate monohydrate was obtained.

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US06747022B2
出典データセットuspto-grants-2004_06
ORD IDord-53137785b67747058d2bdf6f5d0cced2
出典メモuspto-grants-2004_06