反応式
CN([CH:4]=[O:5])C.O[C:7]1[CH:22]=[CH:21][C:10]([C:11](=[O:20])[CH:12]=[CH:13][C:14]2[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=2)=[CH:9][CH:8]=1.[H-].[Na+].ClC[CH2:27][CH2:28][OH:29]>O>[OH:29][CH2:28][CH2:27][CH2:4][O:5][C:17]1[CH:18]=[CH:19][C:14]([CH:13]=[CH:12][C:11]([C:10]2[CH:21]=[CH:22][CH:7]=[CH:8][CH:9]=2)=[O:20])=[CH:15][CH:16]=1参加物
実験手順
A refined 4′-(3-hydroxypropyloxy)-chalcone (9.71 g, 34.4 mmol) was obtained with a yield of 51.4% by adding 90 ml of dry DMF to 4′-hydroxychalcone (15.0 g, 67 mmol) in an air current of argon, and adding sodium hydride (60%, 2.68 g, 67 mmol) through dropping in a reaction flask of 200 ml in ice cooling for 30 minutes; later, after heating to a room temperature and stirring for 5 hours, adding 3-chloro-1-propanol (6.33 g, 67 mmol) through dropping at the same temperature for 10 minutes; furthermore, heating to 80° C., and reacting for 7 hours; next, after injecting the solution into water with ice and extracting the product with ethyl acetate, washing with water, and drying through dehydration with magnesium sulfate, and removing the solvent; after refining (mobile phase, hexane:ethyl acetate=4:1) the gained coarse crystal with silica gel column, recrystallizing with ethyl acetate.
後処理
- waitthrough dropping at the same temperature for 10 minutes
- temperaturefurthermore, heating to 80° C.
- waitreacting for 7 hours
- extractionextracting the product with ethyl acetate
- washwashing with water
- dry with materialdrying through dehydration with magnesium sulfate
- customremoving the solvent
- customrecrystallizing with ethyl acetate
出典と根拠
- ORDレコード
- ord-6313d0c580d9494795cb6dc933f0fa1b
- 出典データセット
- uspto-grants-2002_12
- 特許番号
- US06495221B1
関連ノート
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