반응식
[C:1]1([CH2:7][CH2:8][OH:9])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[CH:10]1(O)[CH2:15][CH2:14][CH2:13][CH2:12][CH2:11]1.S(=O)(=O)(O)O>>[CH:10]1([O:9][CH2:8][CH2:7][C:1]2[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=2)[CH2:15][CH2:14][CH2:13][CH2:12][CH2:11]1참가 물질
4
반응 조건
- 온도
- 115 °C
실험 절차
Into a 2 liter reaction vessel equipped with stirrer, thermometer, heating mantle and overhead condenser with azeotrope takeoff apparatus is placed 488 grams of betaphenylethyl alcohol; 440 grams of cyclohexanol and 100 grams of concentrated sulfuric acid. The reaction mass is then heated to a temperature of 115° C. and maintained at a temperature in the range of 104°-127° C. at reflux while azeotropically removing 80 ml water, for a period of 3 hours. At the end of the 3 hour period, a sample is analyzed by means of GLC analysis (conditions: 180° C. isothermal using an SE-30 packed column). FIG. 1A is the GLC profile of the reaction product at this point.
후처리
- customInto a 2 liter reaction vessel
- customequipped with stirrer
- temperaturethermometer, heating mantle and overhead condenser with azeotrope takeoff apparatus
- temperaturemaintained at a temperature in the range of 104°-127° C.
- temperatureat reflux
- customwhile azeotropically removing 80 ml water
- customAt the end of the 3 hour period
- custom180° C.
출처 및 근거
- ORD 기록
- ord-c657f79a5e5c4bab8f5214e2a6e3b59e
- 출처 데이터셋
- uspto-grants-1981_12
- 특허 번호
- US04306096
연결된 노트
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