反応式
[NH2:1][CH2:2][CH2:3][CH2:4][C:5]([OH:7])=[O:6].C1CCN2C(=NCCC2)CC1.[CH:19]1([N:25]=[C:26]=[O:27])[CH2:24][CH2:23][CH2:22][CH2:21][CH2:20]1.Cl>[OH-].[Na+]>[CH:19]1([NH:25][C:26](=[O:27])[NH:1][CH2:2][CH2:3][CH2:4][C:5]([OH:7])=[O:6])[CH2:24][CH2:23][CH2:22][CH2:21][CH2:20]1参加物
6
実験手順
To a cold solution of 4-aminobutyric acid (2.16 g, 21 mmol) and catalytic amount of DBU in 22 mL of 1.0 N NaOH, 2.5 g (20 mmol) of cyclohexyl isocyanate were added in one time. The mixture was strongly mixed at room temperature overnight. The reaction was then acidified with concentrated HCl. The formed white solid was collected by filtration. The mixture was purified by chromatography on a silica column (8×3 cm). Elution with a mixture 50:50:1 of hexane:ethyl acetate: acetic acid gave the pure targeted product. The resulting white crystal (3.46 g; yield: 76%) had a mp of 153.0-154.0° C. [M+H]+ 281.18.
後処理
- additionThe mixture was strongly mixed at room temperature overnight
- filtrationThe formed white solid was collected by filtration
- customThe mixture was purified by chromatography on a silica column (8×3 cm)
- washElution with a mixture 50:50:1 of hexane
- customethyl acetate: acetic acid gave the pure targeted product
出典と根拠
- ORDレコード
- ord-a5ccf381bfb94412b1c477a5d13b5954
- 出典データセット
- uspto-grants-2010_02
- 特許番号
- US07662910B2
関連ノート
読み込み中…