三碘化硼

反应条件: temp:0.00; pressure:0.00; stir:

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: Subject 2.0 of N-(3,4-dimethoxyphenyl)-1-adamantanecarboxamide and 2.5 g. of boron triiodide to the procedure set forth in Example 6B. Chromatograph the residue obtained thereby on a column containing 35 g. of silica gel using as the eluent a methylene chloride:ethanol: conc. ammonia (90:10:4 v/v). Crystallize the product from chloroform to obtain the product of this Example, m.p. 196°-199°C. Chromatograph the residue obtained on a column containing 35 g Crystallize the product from chloroform to obtain the product of this Example, m.p. 196°-199°C.

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

实验步骤: Subject 2.0 of N-(3,4-dimethoxyphenyl)-1-adamantanecarboxamide and 2.5 g. of boron triiodide to the procedure set forth in Example 6B. Chromatograph the residue obtained thereby on a column containing 35 g. of silica gel using as the eluent a methylene chloride:ethanol: conc. ammonia (90:10:4 v/v). Crystallize the product from chloroform to obtain the product of this Example, m.p. 196°-199°C. Chromatograph the residue obtained on a column containing 35 g Crystallize the product from chloroform to obtain the product of this Example, m.p. 196°-199°C.

反应条件: temp:0.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: Dissolve 3.0 g. of N-(4-methoxybenzyl)-1-adamantanecarboxamide in 25 ml. of methylene chloride and cool the solution to about -78°C. Add 2.6 g. of boron triiodide and allow the reaction mixture to warm up to about 0°C with vigorous stirring. Stir the reaction mixture at about 0°C overnight, then follow the procedure described in Example 6B and crystallize the residue obtained thereby from ethyl acetate to obtain the product of this Example, m.p. 196°-198°C. Dissolve 3.0 g Add 2.6 g crystallize the residue obtained

反应条件: temp:0.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: Dissolve 3.0 g. of N-(4-methoxybenzyl)-1-adamantanecarboxamide in 25 ml. of methylene chloride and cool the solution to about -78°C. Add 2.6 g. of boron triiodide and allow the reaction mixture to warm up to about 0°C with vigorous stirring. Stir the reaction mixture at about 0°C overnight, then follow the procedure described in Example 6B and crystallize the residue obtained thereby from ethyl acetate to obtain the product of this Example, m.p. 196°-198°C. Dissolve 3.0 g Add 2.6 g crystallize the residue obtained

反应条件: temp:0.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: Dissolve 2.0 g. of the product of Step A carboxylate in 15 ml. of methylene chloride and cool the solution to about -78°C. Add 2.5 g. of boron triiodide and allow the reaction mixture to warm up to about 0°C with vigorous stirring. Stir the reaction mixture at about 0°C overnight, then add about 10 ml. saturated sodium bicarbonate solution. Acidify the mixture with 2N hydrochloric acid and extract with ethyl acetate. Decolorize the extract with aqueous sodium thiosulfate, then wash the extract successively with 2N hydrochloric acid solution, saturated sodium bicarbonate solution, and water. Dry the extract over anhydrous sodium sulfate and evaporate to a residue. Crystallize the residue from a toluene-ethanol mixture to obtain the title product 124°C - 126°C. Dissolve 2.0 g Add 2.5 g add about 10 ml extract with ethyl acetate extract with aqueous sodium thiosulfate wash the extract successively with 2N hydrochloric acid solution, saturated sodium bicarbonate solution, and water Dry the extract over anhydrous sodium sulfate evaporate to a residue Crystallize the residue from a toluene-ethanol mixture

反应条件: temp:0.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: Dissolve 2.0 g. of the product of Step A carboxylate in 15 ml. of methylene chloride and cool the solution to about -78°C. Add 2.5 g. of boron triiodide and allow the reaction mixture to warm up to about 0°C with vigorous stirring. Stir the reaction mixture at about 0°C overnight, then add about 10 ml. saturated sodium bicarbonate solution. Acidify the mixture with 2N hydrochloric acid and extract with ethyl acetate. Decolorize the extract with aqueous sodium thiosulfate, then wash the extract successively with 2N hydrochloric acid solution, saturated sodium bicarbonate solution, and water. Dry the extract over anhydrous sodium sulfate and evaporate to a residue. Crystallize the residue from a toluene-ethanol mixture to obtain the title product 124°C - 126°C. Dissolve 2.0 g Add 2.5 g add about 10 ml extract with ethyl acetate extract with aqueous sodium thiosulfate wash the extract successively with 2N hydrochloric acid solution, saturated sodium bicarbonate solution, and water Dry the extract over anhydrous sodium sulfate evaporate to a residue Crystallize the residue from a toluene-ethanol mixture

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

实验步骤: Subject 2.0 g. of N-(3,4-dimethoxyphenyl)-1-adamantanecarboxamide and 2.5 g. of boron triiodide to the procedure set forth in Example 6B. Chromatograph the residue obtained thereby on a column containing 35 g. of silica gel using as the eluent a methylene chloride:ethanol: conc. ammonia (90:10:4 v/v). Crystallize the product from chloroform to obtain the product of this Example, m.p. 196°-199° C. Chromatograph the residue obtained on a column containing 35 g Crystallize the product from chloroform to obtain the product of this Example, m.p. 196°-199° C.

反应条件: temp:0.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: Dissolve 3.0 g. of N-(4-methoxybenzyl)-1-adamantanecarboxamide in 25 ml. of methylene chloride and cool the solution to about -78° C. Add 2.6 g. of boron triiodide and allow the reaction mixture to warm up to about 0° C. with vigorous stirring. Stir the reaction mixture at about 0° C. overnight, then follow the procedure described in Example 6B and crystallize the residue obtained thereby from ethyl acetate to obtain the product of this Example, m.p. 196°-198° C. Dissolve 3.0 g Add 2.6 g crystallize the residue obtained

反应条件: temp:0.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: Dissolve 3.0 g. of N-(4-methoxybenzyl)-1-adamantanecarboxamide in 25 ml. of methylene chloride and cool the solution to about -78° C. Add 2.6 g. of boron triiodide and allow the reaction mixture to warm up to about 0° C. with vigorous stirring. Stir the reaction mixture at about 0° C. overnight, then follow the procedure described in Example 6B and crystallize the residue obtained thereby from ethyl acetate to obtain the product of this Example, m.p. 196°-198° C. Dissolve 3.0 g Add 2.6 g crystallize the residue obtained

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

实验步骤: Subject 2.0 of N-(3,4-dimethoxyphenyl)-1-adamantanecarboxamide and 2.5 g. of boron triiodide to the procedure set forth in Example 6B. Chromatograph the residue obtained thereby on a column containing 35 g. of silica gel using as the eluent a methylene chloride:ethanol: conc. ammonia (90:10:4 v/v). Crystallize the product from chloroform to obtain the product of this Example, m.p. 196°-199°C. Chromatograph the residue obtained on a column containing 35 g Crystallize the product from chloroform to obtain the product of this Example, m.p. 196°-199°C.