Ammonia → 3,3,3-Trifluoro-2,2-dimethyl-propionamide
反応式
[F:1][C:2]([F:10])([F:9])[C:3]([CH3:8])([CH3:7])[C:4](O)=[O:5].C(C1NC=CN=1)(C1[NH:14]C=CN=1)=O.N.C(OCC)C>C(Cl)Cl>[F:1][C:2]([F:10])([F:9])[C:3]([CH3:8])([CH3:7])[C:4]([NH2:14])=[O:5]参加物
6
実験手順
A mixture of 2 g (12.81 mmol) 3,3,3-trifluoro-2,2-dimethylpropionic acid (Aldrich), 2.077 g (12.81 mmol) carbonyl-diimidazole and 5.55 ml (64.1 mmol) aqueous ammonia in 50 ml CH2Cl2 was stirred at room temperature for 20 h. After that, diethyl ether was added and the resulting mixture was washed with 0.1 N HCL, 0.1 N NaOH, water and brine. The organic layer was dried (MgSO4), filtered and concentrated in vacuo to afford 1.15 g of the title compound as white crystals, that were used in the next step without further purification. MS: M+H=156.
後処理
- washthe resulting mixture was washed with 0.1 N HCL, 0.1 N NaOH, water and brine
- dry with materialThe organic layer was dried (MgSO4)
- filtrationfiltered
- concentrationconcentrated in vacuo
出典と根拠
- ORDレコード
- ord-60b2759cdcc14fb2accc5b31f498f7cd
- 出典データセット
- uspto-grants-2013_01
- 特許番号
- US08357707B2
反応ノート
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