反応式
ClC(Cl)(O[C:5](=[O:11])OC(Cl)(Cl)Cl)Cl.[NH2:13][C:14]1[CH:23]=[CH:22][C:21]([C:24]([C:26]2[N:34]3[C:29]([CH:30]=[CH:31][CH:32]=[CH:33]3)=[C:28]([O:35][CH3:36])[C:27]=2[CH3:37])=[O:25])=[CH:20][C:15]=1[C:16](OC)=[O:17].O.[NH2:39][NH2:40].C(N(CC)CC)C>O1CCOCC1.O>[NH2:39][N:40]1[C:16](=[O:17])[C:15]2[C:14](=[CH:23][CH:22]=[C:21]([C:24]([C:26]3[N:34]4[C:29]([CH:30]=[CH:31][CH:32]=[CH:33]4)=[C:28]([O:35][CH3:36])[C:27]=3[CH3:37])=[O:25])[CH:20]=2)[NH:13][C:5]1=[O:11]参加物
反応物 4
生成物 1
試薬・触媒・溶媒 2
実験手順
0.123 g (0.41 mmol) of triphosgene is added, under an inert atmosphere at ambient temperature, to 0.2 g (0.6 mmol) of methyl 2-amino-5-[(1-methoxy-2-methylindolizin-3-yl)carbonyl]benzoate in 10 ml of dioxane. After stirring for 10 minutes, 58 μl (1.2 mmol) of hydrazine hydrate and 0.4 ml (3 mmol) of triethylamine are added. The reaction medium is stirred for 3 hours and then hydrolysed with water. The aqueous phase is extracted with ethyl acetate. The organic phase obtained is dried over sodium sulphate, filtered, and then concentrated under reduced pressure. The solid obtained is purified by silica gel column chromatography, elution being carried out with a dichloromethane/methanol (95/5) mixture. 16 mg of a yellow solid are obtained.
後処理
- stirringThe reaction medium is stirred for 3 hours
- extractionThe aqueous phase is extracted with ethyl acetate
- customThe organic phase obtained
- dry with materialis dried over sodium sulphate
- filtrationfiltered
- concentrationconcentrated under reduced pressure
- customThe solid obtained
- customis purified by silica gel column chromatography, elution
出典と根拠
- ORDレコード
- ord-337cc1c81e154b41b37a65ca2023ad6b
- 出典データセット
- uspto-grants-2014_10
- 特許番号
- US08859544B2
関連ノート
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