N-(4-bromo-2-methoxyphenyl)-2,2,2-trifluoroacetamide

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: Chloroacetone (20 g) was added dropwise to a DMF (160 mL) suspension of N-(4-bromo-2-methoxyphenyl)-2,2,2-trifluoroacetamide (32.4 g), cesium carbonate (71 g) and potassium iodide (1.8 g), and the reaction solution was agitated at room temperature for 2 hours. Then, The reaction solution was stirred for 1 hour and iced water was added thereto. Crystals deposited were separated by filtering. The obtained crystal was suspended in methanol (360 mL) and 2N sodium hydroxide solution (55 mL), and the suspension was agitated for 30 minutes. An iced water was added thereto. Crystals deposited were separated by filtering, and air-dried overnight. 25.2 g of the title compound was obtained. Then, The reaction solution was stirred for 1 hour Crystals deposited were separated by filtering 2N sodium hydroxide solution (55 mL), and the suspension was agitated for 30 minutes An iced water was added Crystals deposited were separated by filtering air-dried overnight

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: Chloroacetone (20 g) was added dropwise to a DMF (160 mL) suspension of N-(4-bromo-2-methoxyphenyl)-2,2,2-trifluoroacetamide (32.4 g), cesium carbonate (71 g) and potassium iodide (1.8 g), and the reaction solution was agitated at room temperature for 2 hours. Then, The reaction solution was stirred for 1 hour and iced water was added thereto. Crystals deposited were separated by filtering. The obtained crystal was suspended in methanol (360 mL) and 2N sodium hydroxide solution (55 mL), and the suspension was agitated for 30 minutes. An iced water was added thereto. Crystals deposited were separated by filtering, and air-dried overnight. 25.2 g of the title compound was obtained. Then, The reaction solution was stirred for 1 hour Crystals deposited were separated by filtering 2N sodium hydroxide solution (55 mL), and the suspension was agitated for 30 minutes An iced water was added Crystals deposited were separated by filtering air-dried overnight

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: Chloroacetone (20 g) was added dropwise to a DMF (160 mL) suspension of N-(4-bromo-2-methoxyphenyl)-2,2,2-trifluoroacetamide (32.4 g), cesium carbonate (71 g) and potassium iodide (1.8 g), and the reaction solution was agitated at room temperature for 2 hours. Then, The reaction solution was stirred for 1 hour and iced water was added thereto. Crystals deposited were separated by filtering. The obtained crystal was suspended in methanol (360 mL) and 2N sodium hydroxide solution (55 mL), and the suspension was agitated for 30 minutes. An iced water was added thereto. Crystals deposited were separated by filtering, and air-dried overnight. 25.2 g of the title compound was obtained. Then, The reaction solution was stirred for 1 hour Crystals deposited were separated by filtering 2N sodium hydroxide solution (55 mL), and the suspension was agitated for 30 minutes An iced water was added Crystals deposited were separated by filtering air-dried overnight

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: Chloroacetone (20 g) was added dropwise to a DMF (160 mL) suspension of N-(4-bromo-2-methoxyphenyl)-2,2,2-trifluoroacetamide (32.4 g), cesium carbonate (71 g) and potassium iodide (1.8 g), and the reaction solution was agitated at room temperature for 2 hours. Then, The reaction solution was stirred for 1 hour and iced water was added thereto. Crystals deposited were separated by filtering. The obtained crystal was suspended in methanol (360 mL) and 2N sodium hydroxide solution (55 mL), and the suspension was agitated for 30 minutes. An iced water was added thereto. Crystals deposited were separated by filtering, and air-dried overnight. 25.2 g of the title compound was obtained. Then, The reaction solution was stirred for 1 hour Crystals deposited were separated by filtering 2N sodium hydroxide solution (55 mL), and the suspension was agitated for 30 minutes An iced water was added Crystals deposited were separated by filtering air-dried overnight

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: Chloroacetone (20 g) was added dropwise to a DMF (160 mL) suspension of N-(4-bromo-2-methoxyphenyl)-2,2,2-trifluoroacetamide (32.4 g), cesium carbonate (71 g) and potassium iodide (1.8 g), and the reaction solution was agitated at room temperature for 2 hours. Then, The reaction solution was stirred for 1 hour and iced water was added thereto. Crystals deposited were separated by filtering. The obtained crystal was suspended in methanol (360 mL) and 2N sodium hydroxide solution (55 mL), and the suspension was agitated for 30 minutes. An iced water was added thereto. Crystals deposited were separated by filtering, and air-dried overnight. 25.2 g of the title compound was obtained. Then, The reaction solution was stirred for 1 hour Crystals deposited were separated by filtering 2N sodium hydroxide solution (55 mL), and the suspension was agitated for 30 minutes An iced water was added Crystals deposited were separated by filtering air-dried overnight