反応式
[CH2:1]([OH:3])[CH3:2].[ClH:4].[CH3:5][O:6][C:7]1[CH:27]=[CH:26][CH:25]=[CH:24][C:8]=1[O:9][CH2:10][CH2:11][CH2:12][CH2:13][CH2:14][O:15][C:16]1[CH:23]=[CH:22][C:19]([C:20]#[N:21])=[CH:18][CH:17]=1>C(OCC)C>[ClH:4].[CH3:5][O:6][C:7]1[CH:27]=[CH:26][CH:25]=[CH:24][C:8]=1[O:9][CH2:10][CH2:11][CH2:12][CH2:13][CH2:14][O:15][C:16]1[CH:17]=[CH:18][C:19]([C:20](=[NH:21])[O:3][CH2:1][CH3:2])=[CH:22][CH:23]=1参加物
反応条件
- 温度
- 5 °C
実験手順
Ethanol (2 B anhydrous, 16.5 L) is cooled with an ice-salt bath to 0° C. Anhydrous hydrogen chloride is introduced until the solution is saturated (~8 hours). At this time the internal temperature is 5° C. To this is added 4-[5-(2-methoxyphenoxy)pentoxy]benzonitrile (1.64 kg, 5.26 mol) as a solid within a period of 10 minutes. At this point additional hydrogen chloride is introduced to maintain saturation at 5° C. for another 8 hours. Almost complete solution is achieved and the color is yellow. The reaction mixture is stirred for a total of 84 hours and the temperature range maintained is 5°-10° C. The resulting slurry is diluted with diethyl ether (52 L) to complete precipitation. The slurry is stirred for 1 hours and filtered. The filter cake is washed with diethyl ether (3×4 L) and air-dried for 1/2 hour to yield ethyl 4-[5-(2-methoxyphenoxy)pentoxy]benzenecarboximidate hydrochloride which is used directly in the next step.
後処理
- custom(~8 hours)
- customis 5° C
- temperaturethe temperature range maintained
- customis 5°-10° C
- customprecipitation
- stirringThe slurry is stirred for 1 hours
- filtrationfiltered
- washThe filter cake is washed with diethyl ether (3×4 L)
- customair-dried for 1/2 hour
出典と根拠
- ORDレコード
- ord-47447b95a1bf45f4834161d3ef59f534
- 出典データセット
- uspto-grants-1993_09
- 特許番号
- US05246965
関連ノート
読み込み中…