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Hexane → (R)-(-)-1-tert-butylcarbonylmethyl-2-oxo-3-amino-5-cyclohexyl-1,3,4,5-tetrahydro-2H-1,5-benzodiazepine oxalate monohydrate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hexane | HCID 8058 | — |
| 反応物 | Oxalic acid dihydrate | HCID 61373 | — |
| 反応物 | (R)-1-tert-butylcarbonylmethyl-2-oxo-3-amino-5-cyclohexyl-1,3,4,5-tetrahydro-2H-1,5-benzodiazepine | HCID 11190074 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | (R)-(-)-1-tert-butylcarbonylmethyl-2-oxo-3-amino-5-cyclohexyl-1,3,4,5-tetrahydro-2H-1,5-benzodiazepine oxalate monohydrate | HCID 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
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06747022B2 |
| 出典データセット | uspto-grants-2004_06 |
| ORD ID | ord-53137785b67747058d2bdf6f5d0cced2 |
| 出典メモ | uspto-grants-2004_06 |