Triethylamine → 1-Aminopiperidine-2,6-dione
反応式
C12(C)C(C)(C)C(CC1)CC2C(Cl)=O.N[CH:15]1[CH2:21][CH2:20][C:19](=[O:22])[NH:18][C:16]1=[O:17].CC[N:25](CC)CC>C(Cl)(Cl)Cl>[NH2:25][N:18]1[C:19](=[O:22])[CH2:20][CH2:21][CH2:15][C:16]1=[O:17]参加物
5
実験手順
A mixture of (+)-camphanic chloride (19 mg, 00868 mmol), aminoglutarimide (21 mg, 0.0868 mmol) and Et3N (24 μl) in CHCl3 (1 ml) was stirred at room for 16 hours. The solution was diluted with CHCl3, washed with saturated aqueous solution of NaHCO3, dried over Na2SO4, concentrated and purified by chromatography (silica gel, CH2Cl2; EtOAc=10:1) to give product (16 mg, 60.0% yield) as a colorless gel: 13CNMR (CDCl3) δ 172.6, 169.4, 168.6; 165.5, 90.3, 58.3, 53.3, 48.2, 47.6, 29.2, 28.2, 26.9, 22.7, 14.6, 7.6; MS (CI/CH4) m/z 308 (M+). This compound exhibited angiogenic activity in the assay of Example 13.
後処理
- washwashed with saturated aqueous solution of NaHCO3
- dry with materialdried over Na2SO4
- concentrationconcentrated
- custompurified by chromatography (silica gel, CH2Cl2; EtOAc=10:1)
出典と根拠
- ORDレコード
- ord-fc361a6e06c64c1fbdbdc621d31d9925
- 出典データセット
- uspto-grants-2014_10
- 特許番号
- US08853253B2
反応ノート
読み込み中…