Phloroglucinol → 3-Methyl-2-nitro-butyric acid ethyl ester
反応式
[N:1]([O-:3])=[O:2].[Na+].C1(C=C(O)C=C(O)C=1)O.[CH2:14]([O:16][C:17](=[O:23])[CH:18](I)[CH:19]([CH3:21])[CH3:20])[CH3:15]>CN(C)C=O>[CH2:14]([O:16][C:17](=[O:23])[CH:18]([N+:1]([O-:3])=[O:2])[CH:19]([CH3:21])[CH3:20])[CH3:15]参加物
5
実験手順
To an ice cooled solution of 5.31 g sodium nitrite and 8 g dried phloroglucinol in 70 ml dimethyl formamide is added a solution of 11.3 g 2-iodo-3-methyl-butyric acid ethyl ester in 30 ml dimethyl formamide. The solution is allowed to warm up to room temperature and is stirred over night. The solvent is removed at reduced pressure. The residue is dissolved in ethyl acetate and washed with water. The organic layer is dried and the solvent is removed. The title compound is obtained as an oil. MS: m/z (M+)=176.1
後処理
- customThe solvent is removed at reduced pressure
- dissolutionThe residue is dissolved in ethyl acetate
- washwashed with water
- customThe organic layer is dried
- customthe solvent is removed
出典と根拠
- ORDレコード
- ord-5d6e3ec387d34890bc6beb155f34c05e
- 出典データセット
- uspto-grants-2013_09
- 特許番号
- US08530493B2
反応ノート
読み込み中…