反応式
[CH3:1][N:2]1[C:6]([CH3:7])=[N:5][N:4]=[N:3]1.C([Li])CCC.[F:13][C:14]1[CH:29]=[C:28]([CH3:30])[CH:27]=[CH:26][C:15]=1[C:16]([C:18]1[CH:23]=[CH:22][C:21]([CH3:24])=[CH:20][C:19]=1[F:25])=[O:17]>O1CCCC1>[F:13][C:14]1[CH:29]=[C:28]([CH3:30])[CH:27]=[CH:26][C:15]=1[C:16]([C:18]1[CH:23]=[CH:22][C:21]([CH3:24])=[CH:20][C:19]=1[F:25])([OH:17])[CH2:7][C:6]1[N:2]([CH3:1])[N:3]=[N:4][N:5]=1参加物
反応条件
- 温度
- -10 °C
実験手順
To a solution of 1,5-dimethyltetrazole (4.6 g, 4.7 mmoles) in tetrahydrofuran (40 mL) at -50° C. was added butyl lithium solution (21.4 mL of a 2.2M solution, 4.7 mmoles). After stirring for 10 minutes, a solution of 2,2'-difluoro-4,4'-dimethylbenzophenone in tetrahydrofuran (15 mL) was added. The solution was stirred for 2.5 hours during which time it was allowed to warm to -10° C. The reaction was quenched by adding 1N hydrochloric acid. The layers were separated and the aqueous layer was extracted with methylene chloride. The combined organic fractions were dried (MgSO4) and evaporated. The residue was triturated with diethyl ether and crystallized from isopropyl acetate to give 8.0 g of the title compound; m.p.=150°-151° C. MS: M+ =344.
後処理
- stirringThe solution was stirred for 2.5 hours during which time it
- customThe reaction was quenched
- additionby adding 1N hydrochloric acid
- customThe layers were separated
- extractionthe aqueous layer was extracted with methylene chloride
- dry with materialThe combined organic fractions were dried (MgSO4)
- customevaporated
- customThe residue was triturated with diethyl ether
- customcrystallized from isopropyl acetate
出典と根拠
- ORDレコード
- ord-6e6ed3e629fa445287a8fa9a3fe0ead4
- 出典データセット
- uspto-grants-1992_05
- 特許番号
- US05110940
関連ノート
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