反応式
[F:1][C:2]([F:22])([F:21])[C:3]1[CH:4]=[C:5]([C:9]2[N:14]3[N:15]=[CH:16][C:17]([C:18]([NH2:20])=[O:19])=[C:13]3[NH:12][CH2:11][CH:10]=2)[CH:6]=[CH:7][CH:8]=1.C([SiH](CC)CC)C.[OH-].[K+]>FC(F)(F)C(O)=O>[F:21][C:2]([F:1])([F:22])[C:3]1[CH:4]=[C:5]([CH:9]2[N:14]3[N:15]=[CH:16][C:17]([C:18]([NH2:20])=[O:19])=[C:13]3[NH:12][CH2:11][CH2:10]2)[CH:6]=[CH:7][CH:8]=1参加物
反応条件
- 温度
- 60 °C
実験手順
A solution of 3.44 g of 4,5-dihydro-7-(3-trifluoromethyl)phenyl)pyrazolo(1,5-a)pyrimidine-3-carboxamide (Example 8) in 40 ml of trifluoroacetic acid is stirred under nitrogen and heated to 60° C. in an oil bath. Then 5.0 ml of triethylsilane is added and the mixture is stirred at 60° C. for 24 hours. The reaction mixture is cooled and carefully poured into a beaker containing a 25 percent aqueous solution of potassium hydroxide and cracked ice. The product which precipitates is extracted into chloroform, and the extract is washed with water, dried over anhydrous sodium sulfate and filtered. The filtrate is evaporated in vacuo to give crystals which are then recrystallized from toluene-hexane to give the desired product, mp 152-154° C.
後処理
- temperatureThe reaction mixture is cooled
- additioncarefully poured into a beaker
- customThe product which precipitates
- extractionis extracted into chloroform
- washthe extract is washed with water
- dry with materialdried over anhydrous sodium sulfate
- filtrationfiltered
- customThe filtrate is evaporated in vacuo
- customto give crystals which
- customare then recrystallized from toluene-hexane
出典と根拠
- ORDレコード
- ord-e7de8176c5cc45b6b607074fc86f9053
- 出典データセット
- uspto-grants-1991_05
- 特許番号
- US05013737
関連ノート
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