Hydrochloric Acid → 1,3-Diazaspiro[4.5]decane-2,4,8-trione
反応式
[NH:1]1[C:5]2([CH2:14][CH2:13][C:8]3(OCC[O:9]3)[CH2:7][CH2:6]2)[C:4](=[O:15])[NH:3][C:2]1=[O:16].Cl>CCO>[NH:1]1[C:5]2([CH2:6][CH2:7][C:8](=[O:9])[CH2:13][CH2:14]2)[C:4](=[O:15])[NH:3][C:2]1=[O:16]参加物
4
実験手順
A suspension of 9,12-dioxa-1,3-diazadispiro[4.2.4.2]tetradecane-2,4-dione (6.33 g, 28.0 mmol) in HCl (6N) (28 mL, 168 mmol) and EtOH (66.0 mL) was stirred at RT for 18 hours. The mixture was partially evaporated (about ½ volume), cooled in an ice bath and brought to a pH of approximately 10. The aqueous layer was extracted with DCM (2×200 mL), and the aqueous layer concentrated. The residue was triturated with THF (2×100 mL), and solids were removed by filtration. The filtrate was evaporated to afford the title compound as a white solid.
後処理
- customThe mixture was partially evaporated (about ½ volume)
- temperaturecooled in an ice bath
- extractionThe aqueous layer was extracted with DCM (2×200 mL)
- concentrationthe aqueous layer concentrated
- customThe residue was triturated with THF (2×100 mL), and solids
- customwere removed by filtration
- customThe filtrate was evaporated
出典と根拠
- ORDレコード
- ord-379aeb423aa94a6ab31f930ee38dfd4f
- 出典データセット
- uspto-grants-2015_08
- 特許番号
- US09115127B2
反応ノート
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