Cyclohexanone → Cyclohexanone, 2-[(4-methoxyphenyl)methylene]-

温度

65 °C

In a 1,000-ml, four-necked flask equipped with a mechanical stirrer, a reflux condenser and a thermometer were placed 68 g (0.5 mole) of p-anisaldehyde, 147 g (1.5 moles) of cyclohexanone and then 200 ml of water slowly. Thereto was slowly added, in a water bath, an aqueous solution obtained by diluting 80 g (0.5 mole) of a 25% aqueous sodium hydroxide solution, with 300 ml of water. The system was stirred at 65° C. for 48 hours and cooled to room temperature. To the system were added 400 ml of toluene and 100 ml of water for phase separation. The aqueous layer was re-extracted with 100 ml of toluene. The toluene layers were combined and washed with water and a saturated aqueous sodium chloride solution in this order. The resulting toluene layer was dried over anhydrous sodium sulfate and subjected to vacuum distillation to remove toluene and the excessive (remaining) cyclohexanone. To the crude oil obtained were added 80 ml of toluene and 80 ml of n-hexane for recrystallization, to obtain 80.4 g of yellow crystals. Yield: 74% The purity of the intended product in the crystals was 88% as measured by high performance liquid chromatography.

1. customIn a 1,000-ml, four-necked flask equipped with a mechanical stirrer, a reflux condenser
2. additionThereto was slowly added, in a water bath
3. customan aqueous solution obtained
4. temperaturecooled to room temperature
5. customfor phase separation
6. extractionThe aqueous layer was re-extracted with 100 ml of toluene
7. washwashed with water
8. dry with materialThe resulting toluene layer was dried over anhydrous sodium sulfate
9. distillationsubjected to vacuum distillation
10. customto remove toluene
11. customTo the crude oil obtained
12. customfor recrystallization

ORDレコード

ord-1a100f660b95437fb00b7c94b235feda

出典データセット

uspto-grants-2010_10

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US07807856B2