Hydrochloric Acid → HCID 23506216、化合物
反応式
COC[O:4][C:5]1[CH:6]=[N:7][CH:8]=[CH:9][C:10]=1[CH2:11][CH2:12][CH2:13][OH:14].Cl>C(O)C>[OH:4][C:5]1[CH:6]=[N:7][CH:8]=[CH:9][C:10]=1[CH2:11][CH2:12][CH2:13][OH:14]参加物
4
実験手順
3-(3-Methoxymethoxypyridin-4-yl)-1-propanol (3.67 g, 18.6 mmol) obtained in Example 2 is dissolved in ethanol (100 ml), and thereto is added a 15% aqueous hydrochloric acid solution (20 ml), and the mixture is heated under reflux for 30 minutes. The reaction solution is concentrated under reduced pressure, and the residue is purified by silica gel column chromatography (eluent: hexane/ethyl acetate), and further recrystallized from diethyl ether to give the title compound (2.08 g) as colorless crystals, m.p. 123-126° C.
後処理
- temperaturethe mixture is heated
- temperatureunder reflux for 30 minutes
- concentrationThe reaction solution is concentrated under reduced pressure
- customthe residue is purified by silica gel column chromatography (eluent: hexane/ethyl acetate)
- customfurther recrystallized from diethyl ether
出典と根拠
- ORDレコード
- ord-706c046adfdc4b8ab13cbe9712942833
- 出典データセット
- uspto-grants-2003_04
- 特許番号
- US06555557B1
反応ノート
読み込み中…