2,2,2-trifluoroethylthiourea

反応条件: temp:0.00; pressure:0.00; stir:

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

実験手順: A solution of 2,2,2-trifluoroethylthiourea (8.0 g.) and methyl iodide (3.5 g.) in EtOH (40 ml.) was heated under reflux for 70 minutes, then evaporated to dryness in vacuo. The residue was triturated with ether to give 2,2,2-trifluoroethyl-S-methylisothiourea hydroiodide, m.p. 154°-156° (90%). under reflux for 70 minutes evaporated to dryness in vacuo The residue was triturated with ether

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

実験手順: A solution of 2,2,2-trifluoroethylthiourea (8.0 g.) and methyl iodide (3.5 g.) in EtOH (40 ml.) was heated under reflux for 70 minutes, then evaporated to dryness in vacuo. The residue was triturated with ether to give 2,2,2-trifluoroethyl-S-methylisothiourea hydroiodide, m.p. 154°-156° (90%). under reflux for 70 minutes evaporated to dryness in vacuo The residue was triturated with ether

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

実験手順: A solution of 2,2,2-trifluoroethylthiourea (8.0 g.) and methyl iodide (3.5 g.) in EtOH (40 ml.) was heated under reflux for 70 minutes, then evaporated to dryness in vacuo. The residue was triturated with ether to give 2,2,2-trifluoroethyl-S-methylisothiourea hydroiodide, m.p. 154°-156° (90%). under reflux for 70 minutes evaporated to dryness in vacuo The residue was triturated with ether

反応条件: temp:0.00; pressure:0.00; stir:

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

実験手順: Slurry 4-cyanophenacyl bromide (1.4 g, 6.3 mmol), 2,2,2-trifluoroethyl-thiourea (1.0 g, 6.3 mmol) and sodium bicarbonate (529 mg, 6.3 mmol) in absolute ethanol (30 mL). Stir the mixture at reflux for 1 h under a nitrogen atmosphere. Cool to room temperature and concentrate in vacuo. Partition the residue between DCM (100 mL) and water (20 mL). Dry the organic layer over Na2SO4 and concentrate in vacuo to obtain the desired intermediate (1.7 g, 95%). MS (ES+) m/z: 284 (M+H)+. at reflux for 1 h under a nitrogen atmosphere concentrate in vacuo Partition the residue between DCM (100 mL) and water (20 mL) Dry the organic layer over Na2SO4 concentrate in vacuo

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

実験手順: Slurry 1-benzoyl-3-(2,2,2-trifluoroethyl)-thiourea (5.5 g, 21.2 mmol) and potassium carbonate (11.7 g, 84.7 mmol) in methanol (180 mL) and water (40 mL). Stir the mixture at room temperature for 16 h. Concentrate the solution in vacuo to a paste. Triturate with hot water (20 mL, 60° C.), filter off the solids, wash with water (20 mL, 25° C.) and hexane (excess). Collect the solids, slurry in EtOAc and concentrate in vacuo twice to remove residual water. Dry the material in a vacuum oven at 45° C. for 16 h to obtain the desired intermediate as an off-white solid (2.2 g, 66%). MS (ES+) m/z: 159.1 (M+H)+. Concentrate the solution in vacuo to a paste Triturate with hot water (20 mL, 60° C.) filter off the solids wash with water (20 mL, 25° C.) and hexane (excess) Collect the solids, slurry in EtOAc concentrate in vacuo twice to remove residual water Dry the material in a vacuum oven at 45° C. for 16 h

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

実験手順: A solution of 2,2,2-trifluoroethylthiourea (8.0 g.) and methyl iodide (3.5 g.) in EtOH (40 ml.) was heated under reflux for 70 minutes, then evaporated to dryness in vacuo. The residue was triturated with ether to give 2,2,2-trifluoroethyl-S-methylisothiourea hydroiodide, m.p. 154°-156° (90%). under reflux for 70 minutes evaporated to dryness in vacuo The residue was triturated with ether

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

実験手順: A solution of 2,2,2-trifluoroethylthiourea (8.0 g.) and methyl iodide (3.5 g.) in EtOH (40 ml.) was heated under reflux for 70 minutes, then evaporated to dryness in vacuo. The residue was triturated with ether to give 2,2,2-trifluoroethyl-S-methylisothiourea hydroiodide, m.p. 154°-156° (90%). under reflux for 70 minutes evaporated to dryness in vacuo The residue was triturated with ether