反応式
C(NC(C)C)(C)C.C([Li])CCC.[Cl:13][C:14]1[CH:15]=[N:16][CH:17]=[C:18]([Cl:20])[CH:19]=1.[C:21](=[O:23])=[O:22]>O1CCCC1.CCCCCC>[Cl:13][C:14]1[CH:15]=[N:16][CH:17]=[C:18]([Cl:20])[C:19]=1[C:21]([OH:23])=[O:22]参加物
反応条件
- 温度
- -70 °C
実験手順
To a solution of 4.96 ml (0.036 mole) of diisopropylamine in 200 ml of tetrahydrofuran at -65° C. under a nitrogen blanket was added dropwise 14.9 ml of 2.5M n-butyllithium in hexane while maintaining the above temperature. Twenty minutes subsequent to that addition, a solution 5.0 g (0.034 mole) of 3,5-dichloropyridine in 30 ml tetrahydrofuran at -60° to -70° C. was added. The reaction mixture was stirred at -70° C. for 1/2 hr, poured onto a large excess of dry ice and allowed to evaporate overnight at room temperature. The residue was taken up in 100 ml of dilute aqueous sodium hydroxide, washed with 3×30 ml of methylenechloride and filtered. The filtrate was acidified to ~pH 2 with dilute hydrochloric acid to precipitate out the product. After cooling, the precipitate was collected and recrystallized from ethyl acetate/hexane giving 1.9 g (29%) of white analytically pure crystals, m.p. 231°-35° C. (decomp.).
後処理
- temperaturewhile maintaining the above temperature
- additionTwenty minutes subsequent to that addition
- customto evaporate overnight at room temperature
- washwashed with 3×30 ml of methylenechloride
- filtrationfiltered
- customto precipitate out the product
- temperatureAfter cooling
- customthe precipitate was collected
- customrecrystallized from ethyl acetate/hexane giving 1.9 g (29%) of white analytically pure crystals, m.p. 231°-35° C. (decomp.)
出典と根拠
- ORDレコード
- ord-f526013860364afd838fa51b7a263463
- 出典データセット
- uspto-grants-1987_02
- 特許番号
- US04642343
関連ノート
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