反応式
[OH:1][C:2]1[CH:12]=[CH:11][C:5]([C:6]([O:8]CC)=[O:7])=[CH:4][CH:3]=1.Br[CH2:14][CH2:15][CH2:16][CH2:17][O:18][CH2:19][C:20]1([CH2:24][CH3:25])[CH2:23][O:22][CH2:21]1>CN(C)C=O>[CH2:24]([C:20]1([CH2:19][O:18][CH2:17][CH2:16][CH2:15][CH2:14][O:1][C:2]2[CH:3]=[CH:4][C:5]([C:6]([OH:8])=[O:7])=[CH:11][CH:12]=2)[CH2:21][O:22][CH2:23]1)[CH3:25]参加物
反応条件
- 温度
- 80 °C
実験手順
In a 300 ml three neck flask, 5.2 g (31 mmol) of ethyl p-hydroxybenzoate, 4.7 g (34 mmol) of potassium carbonate anhydride, and 7.8 g (31 mmol) of the 3-[(4-bromobutoxy)methyl]-3-ethyloxetane were dissolved in 50 ml of dimethylformamide. After the solution remained turbid was heated to a temperature of 80° C. and stirred for 4 hours, the solvent was completely distilled out in a vacuum. To the resulting yellow oily substance were added 15 ml of a 7% sodium hydroxide aqueous solution and 15 ml of methanol. The mixture was refluxed for two and half hours. 1 N (normality) of hydrochloric acid was added to the mixture such that the pH is adjusted to about 3. The resulting white precipitate was filtered and dried in a vacuum thereby obtaining 8.6 g (28 mmol) of 4-[7-(3-ethyl-3-oxetanyl)-1,6-dioxaheptyl]benzoic acid (yield: 89%, identified with 1H-NMR). The resulting compound was no more purified and used in the following reaction.
後処理
- distillationthe solvent was completely distilled out in a vacuum
- additionTo the resulting yellow oily substance were added 15 ml of a 7% sodium hydroxide aqueous solution and 15 ml of methanol
- temperatureThe mixture was refluxed for two and half hours
- addition1 N (normality) of hydrochloric acid was added to the mixture such that the pH
- filtrationThe resulting white precipitate was filtered
- customdried in a vacuum
出典と根拠
- ORDレコード
- ord-e20a963324004b499bf87587735aa884
- 出典データセット
- uspto-grants-2006_08
- 特許番号
- US07087273B2
関連ノート
読み込み中…