反応式
[Cl:1][C:2]1[CH:27]=[CH:26][C:5]2[O:6][C:7]3[CH:25]=[CH:24][CH:23]=[CH:22][C:8]=3[CH2:9][N:10]([C:11]([C:13]3[CH:21]=[CH:20][CH:19]=[CH:18][C:14]=3[C:15](O)=[O:16])=[O:12])[C:4]=2[CH:3]=1.C(OC(Cl)=O)C(C)C.[NH2:36][CH2:37][C:38]1[CH:43]=[CH:42][N:41]=[CH:40][CH:39]=1>C(Cl)Cl>[ClH:1].[Cl:1][C:2]1[CH:27]=[CH:26][C:5]2[O:6][C:7]3[CH:25]=[CH:24][CH:23]=[CH:22][C:8]=3[CH2:9][N:10]([C:11]([C:13]3[CH:21]=[CH:20][CH:19]=[CH:18][C:14]=3[C:15]([NH:36][CH2:37][C:38]3[CH:43]=[CH:42][N:41]=[CH:40][CH:39]=3)=[O:16])=[O:12])[C:4]=2[CH:3]=1参加物
5
反応物 3
生成物 1
試薬・触媒・溶媒 1
実験手順
To a stirred solution of the title product of Example 11 (0.55 g) in CH2Cl2 (10 mL) at 0° C. was added 1-methyl morpholine (0.168 mL) and isobutylchloroformate (0.199 mL) successively. After 30 minutes, 4-(aminomethyl)pyridine (0.156 mL) was added. The mixture was allowed to warm to ambient temperature for hours. The mixture was extracted with ethyl acetate and water. The organic extract was dried over MgSO4 and concentrated. The residue was purified by chromatography over silica gel using ethyl acetate as eluant to give the free base of the title compound as a white solid. The hydrochloride salt of the free base was made in the manner described in Example 3 to give the title compound.
後処理
- extractionThe mixture was extracted with ethyl acetate and water
- extractionThe organic extract
- dry with materialwas dried over MgSO4
- concentrationconcentrated
- customThe residue was purified by chromatography over silica gel
出典と根拠
- ORDレコード
- ord-5cbc34ffa9f54a88b61082ab7fa8a56e
- 出典データセット
- uspto-grants-1995_05
- 特許番号
- US05420270
関連ノート
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