反応式
[NH2:1][C:2]1[N:6]([C:7]2C(Cl)=C[C:10]([C:14]([F:17])([F:16])[F:15])=[CH:9][C:8]=2[Cl:18])[N:5]=[C:4]([C:19]#[N:20])[C:3]=1[S:21][C:22]([F:25])([F:24])[F:23].C(O)C.CC(C)([O-])C.[Na+].CCCCCCC.[C:42]([O:45][CH2:46][CH3:47])(=O)[CH3:43]>CN(C)C=O.[Cu]Br.O>[NH2:1][C:2]1[N:6]([C:7]2[C:42]([O:45][CH2:46][CH3:47])=[CH:43][C:10]([C:14]([F:15])([F:16])[F:17])=[CH:9][C:8]=2[Cl:18])[N:5]=[C:4]([C:19]#[N:20])[C:3]=1[S:21][C:22]([F:25])([F:24])[F:23]参加物
8
反応物 4
生成物 1
試薬・触媒・溶媒 3
反応条件
- 温度
- 90 °C
実験手順
To a mixture of 5-amino-1-(2,6-dichloro-4-trifluoromethylphenyl)-3-cyano-4-trifluoromethylthiopyrazole (4.5 g, 10.7 mmol) and ethanol (0.73 g, 16.0 mmol) in N,N-dimethylformamide (25 ml), was added sodium tert-butoxide (1.54 g, 16.0 mmol) and copper(I)bromide (0.08 g, 0.5 mmol). The mixture was heated at 90° C. for 7 hours under nitrogen. After extractive workup (heptane-ethyl acetate, water) and column chromatography the title product was obtained (2.17 g), mp 166° C., 1H-NMR: 1.34 (3H), 4.14 (2H), 4.35 (2H), 7.20 and 7.45; 19F-NMR: −45.2, −63.9.
出典と根拠
- ORDレコード
- ord-25d93cffb5214c8f898fd5d5e569c14d
- 出典データセット
- uspto-grants-2011_01
- 特許番号
- US07872038B2
関連ノート
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