反应详情

A suspension of compound of example 9 (50 g) and tetrabutylammonium hydrogen sulphate (19.9 g) in DCM is warmed until a homogenous solution is obtained. To this solution benzyl chloride (101 ml) followed by 250 ml of 50% (w/w) NaOH-solution are added. The thick emulsion is refluxed under vigorous stirring. After 1.5 h 12 ml of MeOH is added and the reaction mixture is additionally refluxed for overnight. After cooling it is diluted with 200 ml of DCM and washed with water (400 ml) and brine (100 ml). DCM is evaporated to give a yellow oil (˜150 g) to which 230 ml of MeOH is slowly added. The resulting suspension is stirred overnight at 4° C., the precipitate is filtered, washed with 200 ml of n-heptane and dried i.v. to yield 68 g of white powder. Physical characteristics are in good agreement with those reported [7].

1. temperatureis warmed until a homogenous solution
2. customis obtained
3. additionare added
4. temperatureThe thick emulsion is refluxed under vigorous stirring
5. temperaturethe reaction mixture is additionally refluxed for overnight
6. temperatureAfter cooling it
7. washwashed with water (400 ml) and brine (100 ml)
8. customDCM is evaporated