Ethyl Acetate → HCID 21812870、化合物
反応式
[NH2:1]/[C:2](/[C:6]([CH3:9])([CH3:8])[CH3:7])=[CH:3]\[C:4]#[N:5].O.O.O.O.O.O.O.O.O.O.[S-2:20].[Na+].[Na+].C(OCC)(=O)C>[Cl-].C([N+](CCCC)(CCCC)CCCC)CCC.C1C=CC=CC=1.O>[NH2:1]/[C:2](/[C:6]([CH3:9])([CH3:8])[CH3:7])=[CH:3]\[C:4](=[S:20])[NH2:5]参加物
7
実験手順
(Z)-3-amino-4,4-dimethyl-pent-2-enenitrile (26 g, 209.35 mmol), sodium sulfide decahydrate (5.71 g, 73.27 mmol) and tetrabutyl ammonium chloride (9.31 g, 33.49 mmol) in benzene and water (215 mL, 2.5:1, v/v) is stirred at 75° C. under hydrogen sulfide gas for three days. 200 mL of ethyl acetate is added and the layers separated. The organic layer is washed with water, dried over sodium sulfate, filtered and concentrated under reduced pressure to afford the title compound. Yield 23% over three steps. ESI m/z 159=MH+
後処理
- customthe layers separated
- washThe organic layer is washed with water
- dry with materialdried over sodium sulfate
- filtrationfiltered
- concentrationconcentrated under reduced pressure
出典と根拠
- ORDレコード
- ord-3730f2159afd4d9ebc6d4a3b7243e6e7
- 出典データセット
- uspto-grants-2014_01
- 特許番号
- US08629157B2
反応ノート
読み込み中…