反应详情

BDAM (3.00 grams) was suspended in 30 milliliters of dry CH2Cl2. Two molar equivalents of ether were added dropwise to the chilled suspension. After about 10 minutes of stirring, a homogeneous solution was formed. At this point, 1 molar equivalent of TMAL (1.1 milliliter) was added. The reaction mixture was stirred at room temperature for 15 minutes and 2.00 grams of 4-phenylcyclohexanone were added. Vigorous reflux which quickly subsided was noticed. The reaction mixture was stirred at room temperature for 3 hours and hydrolyzed as described in Example 1. The aqueous layer was acidified to help separate the organic layer. After the usual work up and column separation, 1.75 grams of 4-phenyl-1-methylenecyclohexane were isolated (88% yield).

1. customa homogeneous solution was formed
2. additionAt this point, 1 molar equivalent of TMAL (1.1 milliliter) was added
3. stirringThe reaction mixture was stirred at room temperature for 15 minutes
4. temperatureVigorous reflux which
5. stirringThe reaction mixture was stirred at room temperature for 3 hours
6. customto help separate the organic layer
7. customAfter the usual work up and column separation