苯甲酮二甲基缩酮

反应条件: temp:27.51; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: In a round bottom flask, (12 g) 3-hydroxy-2-(hydroxymethyl)-2-methylpropanoic acid and 35 ml toluene was taken. (99.4 mg) p-toluene sulfonic acid was added into the reaction mixture at 25-30° C. temperature. The reaction mixture was heated at reflux temperature, and 20.5 g (1 equiv.) dimethoxy diphenylmethane [IIa3] in 35 ml toluene was added and it was further refluxed under dean stark. Continuous removal and addition of toluene done upto 3 hrs. Then reaction mixture was cooled at 25-30° C. and dumped into water. The reaction mixture was stirred at 20-30° C. and filter it and wash the solid mass with water to obtain white solid product. The reaction mixture was heated was added it was further refluxed under dean stark Continuous removal and addition of toluene Then reaction mixture filter it wash the solid mass with water to obtain white solid product

反应条件: temp:27.51; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: In a round bottom flask, (10 g) Benzophenone in 20 ml methanol was taken. 12 ml (2 equiv.) trimethyl orthoformate was added into the reaction mixture in a single lot and the reaction mixture was stirred at 25-30° C. 3-4 drop perchloric acid (HClO4 as a catalyst) was added and reflux it for 9 hr. After completion of the reaction, the reaction mass was dumped into water. Subsequently, the reaction mass was stirred for 15 min, filtered it and wash the solid mass with water to obtain white solid product. reflux it for 9 hr After completion of the reaction Subsequently, the reaction mass was stirred for 15 min filtered it wash the solid mass with water to obtain white solid product

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

实验步骤: 3-Mercapto-1,2-propanediol(3.26 g, 30.00 mmol) was dissolved in benzene (60 mL). Benzophenone dimethyl ketal (13.48 g, 60.0 mmol, 2 equiv.) and CSA (0.70 mg, 3.00 mmol, 0.1 equiv.) were added. The solution was heated with an oil bath to reflux. Benzene/methanol was collected and removed while more benzene was added to the refluxing reaction. After about 200 mL benzene/methanol was distilled out, the reaction was cooled to room temperature, applied directly onto a silica gel column. The column was then eluted was 20%-40% ether/petroleum ether to afford a thick oil as the desired product (3.78 g, 46). Rf=0.25, 20% ether/petroleum ether. 1H NMR (400 MHz, C6D6) δ=2.56 (dd, J=6.3, 10.2 Hz, 1 H), 2.83 (dd, J=7.7, 10.2 Hz, 1 H), 3.35 (br dd, J=5.3, 11.6 Hz, 1 H), 3.44 (br dd, J=3.5, 11.6 Hz, 1 H), 3.88-3.95 (m, 1 H), 6.94-7.20 (m, 6H), 7.54 (d, J=7.5 Hz, 2 H), 7.70 (d, J=7.5 Hz, 2 H). 13C NMR (100 MHz, C6D6) δ=35.90, 63.97, 83.29, 100.20, 126-129 (m). The solution was heated with an oil bath to reflux Benzene/methanol was collected removed while more benzene was added to the refluxing reaction After about 200 mL benzene/methanol was distilled out The column was then eluted

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

实验步骤: 3-Mercapto-1,2-propanediol(3.26 g, 30.00 mmol) was dissolved in benzene (60 mL). Benzophenone dimethyl ketal (13.48 g, 60.0 mmol, 2 equiv.) and CSA (0.70 mg, 3.00 mmol, 0.1 equiv.) were added. The solution was heated with an oil bath to reflux. Benzene/methanol was collected and removed while more benzene was added to the refluxing reaction. After about 200 mL benzene/methanol was distilled out, the reaction was cooled to room temperature, applied directly onto a silica gel column. The column was then eluted was 20%-40% ether/petroleum ether to afford a thick oil as the desired product (3.78 g, 46). Rf =0.25, 20% ether/petroleum ether. 1H NMR (400 MHz, C6D6) δ=2.56 (dd, J=6.3, 10.2 Hz, 1H), 2.83 (dd, J=7.7, 10.2 Hz, 1H), 3.35 (br dd, J=5.3, 11.6 Hz, 1H), 3.44 (br dd, J=3.5, 11.6 Hz, 1H), 3.88-3.95 (m, 1H), 6.94-7.20 (m, 6H), 7.54 (d, J=7.5 Hz, 2H), 7.70 (d, J=7.5 Hz, 2H). 13C NMR (100 MHz, C6D6) δ=35.90, 63.97, 83.29, 100.20, 126-129 (m). The solution was heated with an oil bath to reflux Benzene/methanol was collected removed while more benzene was added to the refluxing reaction After about 200 mL benzene/methanol was distilled out The column was then eluted

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

实验步骤: 3-Mercapto-1,2-propanediol(3.26 g, 30.00 mmol) was dissolved in benzene (60 mL). Benzophenone dimethyl ketal (13.48 g, 60.0 mmol, 2 equiv.) and CSA (0.70 mg, 3.00 mmol, 0.1 equiv.) were added. The solution was heated with an oil bath to reflux. Benzene/methanol was collected and removed while more benzene was added to the refluxing reaction. After about 200 mL benzene/methanol was distilled out, the reaction was cooled to room temperature, applied directly onto a silica gel column. The column was then eluted was 20%-40% etherlpetroleum ether to afford a thick oil as the desired product (3.78 g, 46). Rf =0.25, 20% ether/petroleum ether. 1H NMR (400 MIHz, C6D6) δ=2.56 (dd, J 6.3, 10.2 Hz, 1 H), 2.83 (dd, J=7.7, 10.2 Hz, 1 H), 3.35 (br dd, J=5.3, 11.6 Hz, 1 H), 3.44 (br dd, J=3.5, 11.6 Hz, 1 H), 3.88-3.95 (m, 1 H), 6.94-7.20 (m, 6H), 7.54 (d, J=7.5 Hz, 2 H), 7.70 (d, J=7.5 Hz, 2 H). 13C NMR (100 MHz, C6D6) δ=35.90, 63.97, 83.29, 100.20, 126-129 (m). The solution was heated with an oil bath to reflux Benzene/methanol was collected removed while more benzene was added to the refluxing reaction After about 200 mL benzene/methanol was distilled out The column was then eluted

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

实验步骤: 3-Mercapto-1,2-propanediol(3.26 g, 30.00 mmol) was dissolved in benzene (60 mL). Benzophenone dimethyl ketal (13.48 g, 60.0 mmol, 2 equiv.) and CSA (0.70 mg, 3.00 mmol, 0.1 equiv.) were added. The solution was heated with an oil bath to reflux. Benzene/methanol was collected and removed while more benzene was added to the refluxing reaction. After about 200 mL benzene/methanol was distilled out, the reaction was cooled to room temperature, applied directly onto a silica gel column. The column was then eluted was 20%-40% etherlpetroleum ether to afford a thick oil as the desired product (3.78 g, 46). Rf =0.25, 20% ether/petroleum ether. 1H NMR (400 MIHz, C6D6) δ=2.56 (dd, J 6.3, 10.2 Hz, 1 H), 2.83 (dd, J=7.7, 10.2 Hz, 1 H), 3.35 (br dd, J=5.3, 11.6 Hz, 1 H), 3.44 (br dd, J=3.5, 11.6 Hz, 1 H), 3.88-3.95 (m, 1 H), 6.94-7.20 (m, 6H), 7.54 (d, J=7.5 Hz, 2 H), 7.70 (d, J=7.5 Hz, 2 H). 13C NMR (100 MHz, C6D6) δ=35.90, 63.97, 83.29, 100.20, 126-129 (m). The solution was heated with an oil bath to reflux Benzene/methanol was collected removed while more benzene was added to the refluxing reaction After about 200 mL benzene/methanol was distilled out The column was then eluted

反应条件: temp:27.51; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: In a round bottom flask, (12 g) 3-hydroxy-2-(hydroxymethyl)-2-methylpropanoic acid and 35 ml toluene was taken. (99.4 mg) p-toluene sulfonic acid was added into the reaction mixture at 25-30° C. temperature. The reaction mixture was heated at reflux temperature, and 20.5 g (1 equiv.) dimethoxy diphenylmethane [IIa3] in 35 ml toluene was added and it was further refluxed under dean stark. Continuous removal and addition of toluene done upto 3 hrs. Then reaction mixture was cooled at 25-30° C. and dumped into water. The reaction mixture was stirred at 20-30° C. and filter it and wash the solid mass with water to obtain white solid product. The reaction mixture was heated was added it was further refluxed under dean stark Continuous removal and addition of toluene Then reaction mixture filter it wash the solid mass with water to obtain white solid product

反应条件: temp:27.51; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: In a round bottom flask, (12 g) 3-hydroxy-2-(hydroxymethyl)-2-methylpropanoic acid and 35 ml toluene was taken. (99.4 mg) p-toluene sulfonic acid was added into the reaction mixture at 25-30° C. temperature. The reaction mixture was heated at reflux temperature, and 20.5 g (1 equiv.) dimethoxy diphenylmethane [IIa3] in 35 ml toluene was added and it was further refluxed under dean stark. Continuous removal and addition of toluene done upto 3 hrs. Then reaction mixture was cooled at 25-30° C. and dumped into water. The reaction mixture was stirred at 20-30° C. and filter it and wash the solid mass with water to obtain white solid product. The reaction mixture was heated was added it was further refluxed under dean stark Continuous removal and addition of toluene Then reaction mixture filter it wash the solid mass with water to obtain white solid product

反应条件: temp:27.51; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: In a round bottom flask, (10 g) Benzophenone in 20 ml methanol was taken. 12 ml (2 equiv.) trimethyl orthoformate was added into the reaction mixture in a single lot and the reaction mixture was stirred at 25-30° C. 3-4 drop perchloric acid (HClO4 as a catalyst) was added and reflux it for 9 hr. After completion of the reaction, the reaction mass was dumped into water. Subsequently, the reaction mass was stirred for 15 min, filtered it and wash the solid mass with water to obtain white solid product. reflux it for 9 hr After completion of the reaction Subsequently, the reaction mass was stirred for 15 min filtered it wash the solid mass with water to obtain white solid product

反应条件: temp:27.51; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: In a round bottom flask, (10 g) Benzophenone in 20 ml methanol was taken. 12 ml (2 equiv.) trimethyl orthoformate was added into the reaction mixture in a single lot and the reaction mixture was stirred at 25-30° C. 3-4 drop perchloric acid (HClO4 as a catalyst) was added and reflux it for 9 hr. After completion of the reaction, the reaction mass was dumped into water. Subsequently, the reaction mass was stirred for 15 min, filtered it and wash the solid mass with water to obtain white solid product. reflux it for 9 hr After completion of the reaction Subsequently, the reaction mass was stirred for 15 min filtered it wash the solid mass with water to obtain white solid product

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

实验步骤: 3-Mercapto-1,2-propanediol(3.26 g, 30.00 mmol) was dissolved in benzene (60 mL). Benzophenone dimethyl ketal (13.48 g, 60.0 mmol, 2 equiv.) and CSA (0.70 mg, 3.00 mmol, 0.1 equiv.) were added. The solution was heated with an oil bath to reflux. Benzene/methanol was collected and removed while more benzene was added to the refluxing reaction. After about 200 mL benzene/methanol was distilled out, the reaction was cooled to room temperature, applied directly onto a silica gel column. The column was then eluted was 20%-40% ether/petroleum ether to afford a thick oil as the desired product (3.78 g, 46). Rf=0.25, 20% ether/petroleum ether. 1H NMR (400 MHz, C6D6) δ=2.56 (dd, J=6.3, 10.2 Hz, 1 H), 2.83 (dd, J=7.7, 10.2 Hz, 1 H), 3.35 (br dd, J=5.3, 11.6 Hz, 1 H), 3.44 (br dd, J=3.5, 11.6 Hz, 1 H), 3.88-3.95 (m, 1 H), 6.94-7.20 (m, 6H), 7.54 (d, J=7.5 Hz, 2 H), 7.70 (d, J=7.5 Hz, 2 H). 13C NMR (100 MHz, C6D6) δ=35.90, 63.97, 83.29, 100.20, 126-129 (m). The solution was heated with an oil bath to reflux Benzene/methanol was collected removed while more benzene was added to the refluxing reaction After about 200 mL benzene/methanol was distilled out The column was then eluted

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

实验步骤: 3-Mercapto-1,2-propanediol(3.26 g, 30.00 mmol) was dissolved in benzene (60 mL). Benzophenone dimethyl ketal (13.48 g, 60.0 mmol, 2 equiv.) and CSA (0.70 mg, 3.00 mmol, 0.1 equiv.) were added. The solution was heated with an oil bath to reflux. Benzene/methanol was collected and removed while more benzene was added to the refluxing reaction. After about 200 mL benzene/methanol was distilled out, the reaction was cooled to room temperature, applied directly onto a silica gel column. The column was then eluted was 20%-40% ether/petroleum ether to afford a thick oil as the desired product (3.78 g, 46). Rf =0.25, 20% ether/petroleum ether. 1H NMR (400 MHz, C6D6) δ=2.56 (dd, J=6.3, 10.2 Hz, 1H), 2.83 (dd, J=7.7, 10.2 Hz, 1H), 3.35 (br dd, J=5.3, 11.6 Hz, 1H), 3.44 (br dd, J=3.5, 11.6 Hz, 1H), 3.88-3.95 (m, 1H), 6.94-7.20 (m, 6H), 7.54 (d, J=7.5 Hz, 2H), 7.70 (d, J=7.5 Hz, 2H). 13C NMR (100 MHz, C6D6) δ=35.90, 63.97, 83.29, 100.20, 126-129 (m). The solution was heated with an oil bath to reflux Benzene/methanol was collected removed while more benzene was added to the refluxing reaction After about 200 mL benzene/methanol was distilled out The column was then eluted