反応式
[O:1]1[CH2:5][CH2:4][C:3]([C:6]2[C:12]([CH3:13])=[CH:11][CH:10]=[CH:9][C:7]=2N)=[N:2]1.N(OCCCC)=O.[CH3:21][S:22]C>[Cu](Cl)Cl>[CH3:13][C:12]1[CH:11]=[CH:10][CH:9]=[C:7]([S:22][CH3:21])[C:6]=1[C:3]1[CH2:4][CH2:5][O:1][N:2]=1参加物
5
反応条件
- 温度
- 60 °C
実験手順
25 g (0.14 mol) of 2-(4,5-dihydroisoxazol-3-yl)-3-methylaniline and 0.2 g of copper(II) chloride are initially charged in 200 ml of dimethyl sulfide, and 16.1 g of n-butyl nitrite (0.15 mol) are added dropwise at 55-62° C. The mixture is then stirred at 60° C. for 0.5 hours. For work-up, the mixture is then washed with dilute hydrochloric acid and water and then concentrated under reduced pressure. This gives 26.3 g (91%) of a dark oil which solidifies after a while (content according to HPLC 96%). The product can be purified further by trituration with methyl tert-butyl ether.
後処理
- washFor work-up, the mixture is then washed with dilute hydrochloric acid and water
- concentrationconcentrated under reduced pressure
- customThe product can be purified further by trituration with methyl tert-butyl ether
出典と根拠
- ORDレコード
- ord-4667484a23334ebf815b0c9efb18c0e8
- 出典データセット
- uspto-grants-2004_03
- 特許番号
- US06706886B2
関連ノート
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