NSC30272

反应条件: temp:100.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: A mixture of 30.6 g (0.149 mol) of 1,3-dichloro-2-phenylpropan-2-ol, 55.5 g (0.300 mol) of potassium phthalimide and 300 ml of dimethylformamide is heated in a water bath at 100° C. for 4 h. The resulting reaction medium is cooled and evaporated until the volume has been halved, and the insoluble material formed is filtered off, washed with CH3OH and then dried to give 40 g (yield: 63%) of 1,3-diphthalimido-2-phenylpropan-2-ol. The resulting reaction medium is cooled evaporated until the volume the insoluble material formed is filtered off washed with CH3OH dried

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: 289 ml (0.866 mol) of a 3M solution of phenylmagnesium bromide in ether are run, over a period of 1.50 h, into a solution of 100 g (0.787 mol) of 1,3-dichloroacetone in 1000 ml of anhydrous ether under a nitrogen atmosphere and at -60° C. After 10 minutes, a solution of 83.5 g of acetic acid in 126 ml of ether is added to the reaction medium. The temperature is allowed to rise to +4° C. and 315 ml of water are run in. The ether phase is decanted, washed with water and dried over MgSO4. It is filtered, the filtrate is evaporated to dryness and the evaporation residue is distilled in vacuo to give 82.3 g (yield: 51%) of 1,3-dichloro-2-phenylpropan-2-ol. B.p. (0.5 mm Hg)=102° C. (0.5 mm Hg corresponds to 66.6 Pa). to rise to +4° C. The ether phase is decanted washed with water dried over MgSO4 It is filtered the filtrate is evaporated to dryness the evaporation residue is distilled in vacuo

反应条件: temp:100.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: A mixture of 30.6 g (0.149 mol) of 1,3-dichloro-2-phenylpropan-2-ol, 55.5 g (0.300 mol) of potassium phthalimide and 300 ml of dimethylformamide is heated in a water bath at 100° C. for 4 h. The resulting reaction medium is cooled and evaporated until the volume has been halved, and the insoluble material formed is filtered off, washed with CH3OH and then dried to give 40 g (yield: 63%) of 1,3-diphthalimido-2-phenylpropan-2-ol. The resulting reaction medium is cooled evaporated until the volume the insoluble material formed is filtered off washed with CH3OH dried

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: 289 ml (0.866 mol) of a 3M solution of phenylmagnesium bromide in ether are run, over a period of 1.50 h, into a solution of 100 g (0.787 mol) of 1,3-dichloroacetone in 1000 ml of anhydrous ether under a nitrogen atmosphere and at -60° C. After 10 minutes, a solution of 83.5 g of acetic acid in 126 ml of ether is added to the reaction medium. The temperature is allowed to rise to +4° C. and 315 ml of water are run in. The ether phase is decanted, washed with water and dried over MgSO4. It is filtered, the filtrate is evaporated to dryness and the evaporation residue is distilled in vacuo to give 82.3 g (yield: 51%) of 1,3-dichloro-2-phenylpropan-2-ol. B.p. (0.5 mm Hg)=102° C. (0.5 mm Hg corresponds to 66.6 Pa). to rise to +4° C. The ether phase is decanted washed with water dried over MgSO4 It is filtered the filtrate is evaporated to dryness the evaporation residue is distilled in vacuo