甲基3,3,3-三氟-2-羟基-2-三氟丙酸甲酯

反应条件: temp:0.00; pressure:0.00; stir:

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

实验步骤: To a mixture of 25.0 g of sodium boron hydride, 500 g of water, and 500 g of diethyl ether, with stirring, 100 g of methyl 2-hydroxy-3,3,3-trifluoro-2-trifluoromethylpropionate was added dropwise. The mixture was stirred for 10 hours, after which hydrochloric acid was added to quench the reaction. An organic layer was separated from the reaction mixture, concentrated, and distilled, obtaining 83.9 g of 3,3,3-trifluoro-2-trifluoromethyl-1,2-propane diol (yield 96%). The mixture was stirred for 10 hours to quench the reaction An organic layer was separated from the reaction mixture concentrated distilled

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

实验步骤: To a mixture of 25.0 g of sodium boron hydride, 500 g of water, and 500 g of diethyl ether, with stirring, 100 g of methyl 2-hydroxy-3,3,3-trifluoro-2-trifluoromethylpropionate was added dropwise. The mixture was stirred for 10 hours, after which hydrochloric acid was added to quench the reaction. An organic layer was separated from the reaction mixture, concentrated, and distilled, obtaining 83.9 g of 3,3,3-trifluoro-2-trifluoromethyl-1,2-propane diol (yield 96%). The mixture was stirred for 10 hours to quench the reaction An organic layer was separated from the reaction mixture concentrated distilled

反应条件: temp:60.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: A flask was charged with 9.7 g of magnesium and 200 ml of tetrahydrofuran, to which 43.2 g of 1,4-dibromobutane was added dropwise at 60° C. After the completion of dropwise addition, the contents were stirred for one hour at 60° C., and 22.6 g of methyl 2-hydroxy-3,3,3-trifluoro-2-trifluoromethylpropionate was added dropwise below 50° C. The mixture was stirred for one hour at room temperature, after which an ammonium chloride aqueous solution was added. This was followed by ordinary work-up and vacuum distillation, obtaining 22.4 g of the target compound (yield 89%). was added dropwise at 60° C After the completion of dropwise addition The mixture was stirred for one hour at room temperature This was followed by ordinary work-up and vacuum distillation

反应条件: temp:60.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: A flask was charged with 9.7 g of magnesium and 200 ml of tetrahydrofuran, to which 43.2 g of 1,4-dibromobutane was added dropwise at 60° C. After the completion of dropwise addition, the contents were stirred for one hour at 60° C., and 22.6 g of methyl 2-hydroxy-3,3,3-trifluoro-2-trifluoromethylpropionate was added dropwise below 50° C. The mixture was stirred for one hour at room temperature, after which an ammonium chloride aqueous solution was added. This was followed by ordinary work-up and vacuum distillation, obtaining 22.4 g of the target compound (yield 89%). was added dropwise at 60° C After the completion of dropwise addition The mixture was stirred for one hour at room temperature This was followed by ordinary work-up and vacuum distillation

反应条件: temp:60.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: A flask was charged with 9.5 g of magnesium and 300 ml of tetrahydrofuran, to which 35.0 g of isopropyl chloride was added dropwise at 50° C. After the completion of dropwise addition, the contents were stirred for one hour at 60° C., and 22.6 g of methyl 2-hydroxy-3,3,3-trifluoro-2-trifluoromethylpropionate was added dropwise below 50° C. The mixture was stirred for one hour at room temperature, after which an ammonium chloride aqueous solution was added. This was followed by ordinary work-up and vacuum distillation, obtaining 20.2 g of the target compound (yield 84%). was added dropwise at 50° C After the completion of dropwise addition The mixture was stirred for one hour at room temperature This was followed by ordinary work-up and vacuum distillation

反应条件: temp:60.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: A flask was charged with 9.5 g of magnesium and 300 ml of tetrahydrofuran, to which 35.0 g of isopropyl chloride was added dropwise at 50° C. After the completion of dropwise addition, the contents were stirred for one hour at 60° C., and 22.6 g of methyl 2-hydroxy-3,3,3-trifluoro-2-trifluoromethylpropionate was added dropwise below 50° C. The mixture was stirred for one hour at room temperature, after which an ammonium chloride aqueous solution was added. This was followed by ordinary work-up and vacuum distillation, obtaining 20.2 g of the target compound (yield 84%). was added dropwise at 50° C After the completion of dropwise addition The mixture was stirred for one hour at room temperature This was followed by ordinary work-up and vacuum distillation

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

实验步骤: To a mixture of 25.0 g of sodium boron hydride, 500 g of water, and 500 g of diethyl ether, with stirring, 100 g of methyl 2-hydroxy-3,3,3-trifluoro-2-trifluoromethylpropionate was added dropwise. The mixture was stirred for 10 hours, after which hydrochloric acid was added to quench the reaction. An organic layer was separated from the reaction mixture, concentrated, and distilled, obtaining 83.9 g of 3,3,3-trifluoro-2-trifluoromethyl-1,2-propane diol (yield 96%). The mixture was stirred for 10 hours to quench the reaction An organic layer was separated from the reaction mixture concentrated distilled

反应条件: temp:60.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: A flask was charged with 9.7 g of magnesium and 200 ml of tetrahydrofuran, to which 43.2 g of 1,4-dibromobutane was added dropwise at 60° C. After the completion of dropwise addition, the contents were stirred for one hour at 60° C., and 22.6 g of methyl 2-hydroxy-3,3,3-trifluoro-2-trifluoromethylpropionate was added dropwise below 50° C. The mixture was stirred for one hour at room temperature, after which an ammonium chloride aqueous solution was added. This was followed by ordinary work-up and vacuum distillation, obtaining 22.4 g of the target compound (yield 89%). was added dropwise at 60° C After the completion of dropwise addition The mixture was stirred for one hour at room temperature This was followed by ordinary work-up and vacuum distillation

反应条件: temp:60.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: A flask was charged with 9.5 g of magnesium and 300 ml of tetrahydrofuran, to which 35.0 g of isopropyl chloride was added dropwise at 50° C. After the completion of dropwise addition, the contents were stirred for one hour at 60° C., and 22.6 g of methyl 2-hydroxy-3,3,3-trifluoro-2-trifluoromethylpropionate was added dropwise below 50° C. The mixture was stirred for one hour at room temperature, after which an ammonium chloride aqueous solution was added. This was followed by ordinary work-up and vacuum distillation, obtaining 20.2 g of the target compound (yield 84%). was added dropwise at 50° C After the completion of dropwise addition The mixture was stirred for one hour at room temperature This was followed by ordinary work-up and vacuum distillation

反应条件: temp:0.00; pressure:0.00; stir:

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

实验步骤: Synthesis was carried out in accordance with the procedure described in U.S. Pat. No. 7,868,199. In a nitrogen atmosphere, 84 g of sodium boron hydride, 1,450 g of diisopropyl ether (IPE), 2,000 g of water and 1.7 g of 25 wt % NaOH aqueous solution were ice cooled, to which 500 g of methyl 3,3,3-trifluoro-2-hydroxy-2-(trifluoromethyl)propanoate was added dropwise. Stirring was continued for 24 hours at room temperature. Under ice cooling, 444 g of 20 wt % hydrochloric acid aqueous solution was added dropwise to quench the reaction. After the water layer was removed, the organic layer was washed with water and concentrated at 50° C. and a slightly reduced pressure of 6.7 kPa, obtaining 682 g of a 61 wt % IPE solution of 3,3,3-trifluoro-2-trifluoromethyl-1,2-propane diol (yield 95%). The compound was used in the subsequent reaction without further purification. Synthesis was added dropwise to quench the reaction After the water layer was removed the organic layer was washed with water concentrated at 50° C.