反応式
[C:1](=[O:14])([O:3][C:4]12[CH2:13][CH:8]3[CH2:9][CH:10]([CH2:12][CH:6]([CH2:7]3)[CH2:5]1)[CH2:11]2)[NH2:2].IC1C=CC=C(CC([O-])=O)C=1CC([O-])=O.[O-2].[Mg+2]>ClCCl.CC(O)=O.CC(O)=O.CC(O)=O.CC(O)=O.[Rh].[Rh]>[C:4]123[CH2:5][CH:6]4[CH2:12][CH:10]([CH2:9][CH:8]([CH2:7]4)[CH:13]1[NH:2][C:1](=[O:14])[O:3]2)[CH2:11]3参加物
6
実験手順
Tricyclo[3.3.1.13,7]dec-1-yl carbamate (100 mg, 0.512 mmol), iodobenzenediacetate (220 mg, 0.683 mmol), magnesium oxide (50 mg, 1.24 mmol) and rhodium (II) acetate dimer (22 mg, 0.050 mmol) were stirred in dichloromethane (3 mL) at 50° C. for 5 hours. After completion of the reaction, the reaction solution was filtered, and the solid was washed with chloroform and the filtrate was evaporated under reduced pressure. The resulting residue was purified by silica gel column chromatography (hexane/ethyl acetate=10/1→2/1) to give the desired product (77% yield).
後処理
- customAfter completion of the reaction
- filtrationthe reaction solution was filtered
- washthe solid was washed with chloroform
- customthe filtrate was evaporated under reduced pressure
- customThe resulting residue was purified by silica gel column chromatography (hexane/ethyl acetate=10/1→2/1)
出典と根拠
- ORDレコード
- ord-d4ce184fdb4f48e6b71ded0bd1b8f1ab
- 出典データセット
- uspto-grants-2013_05
- 特許番号
- US08440666B2
関連ノート
読み込み中…