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]SC>[Cu]>[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
40 g (0.22 mol) of 2-(4,5-dihydroisoxazol-3-yl)-3-methylaniline and 1.5 g of copper powder are initially charged in 300 ml of dimethyl disulfide, and 26.1 g of n-butyl nitrite (0.23 mol) are added dropwise at 55-66° C. The mixture is then stirred at 60° C. for 1.5 hours. For work-up, the hot mixture is filtered through activated carbon and then washed with dilute hydrochloric acid and water and then concentrated under reduced pressure. This gives 44.5 g (88%) of a dark oil which solidifies after a while (content according to HPLC (95%). The product can be purified further by trituration with methyl tert-butyl ether.
後処理
- filtrationFor work-up, the hot mixture is filtered through activated carbon
- washwashed 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-10d7ee252c7444df9fec62dd0a3dc293
- 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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