反应详情

In 40 ml of a 5% sodium hydroxide solution 5.2 g (20 -millimoles) of 6-hydroxy-7-sec. butoxy-2,2-dimethyl-4-chromanone are dissolved whereupon 80 ml of dichloro methane and 0.5 g of triethyl benzyl ammonium chloride are added and the mixture is intensively stirred at room temperature for 30 minutes. After the addition of 4.25 g (1.9 ml, 30 millimoles) of methyl iodide the reaction mixture is stirred for another 2 hours. The organic phase is separated, washed twice with 50 ml of water each, dried over sodium sulfate and the solvent is removed. The residue is crystallized from 90% ethanol. Thus 5.34 g of the desired compound are obtained, yield 96%. Mp.: 92.5°-93° C.

1. additionare added
2. stirringis stirred for another 2 hours
3. customThe organic phase is separated
4. washwashed twice with 50 ml of water each,
5. dry with materialdried over sodium sulfate
6. customthe solvent is removed
7. customThe residue is crystallized from 90% ethanol