methylcarbamothioylsulfanyl N-methylcarbamodithioate

反応条件: temp:0.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: In a 4-litter bottle equipped with a mechanical stirrer, sodium hydroxide (80 g, 2 mol) was dissolved in water (500 mL) and the solution was cooled to 0° C. (ice-water bath). THF (200 mL), methylamine (40% in water, 170 mL, 2 mol) and carbon disulfide (120 mL, 2 mol) were added and the mixture as stirred at 0° C. for 30 minutes. Crushed ice (1.5 kg) was added, followed by glacial acetic acid (300 mL). Hydrogen peroxide (30%, 100 mL, 1 mol) was added dropwise over 10 minutes with temperature maintained below 50° C. by adding ice with stirring. Hexanes (or heptane) (800 mL) was added and the mixture was stirred for another 30 minutes in an ice-water bath. The mixture was filtered and washed with aqueous trichloroacetic acid (2%, 5×200 mL) and hexanes (or heptane) (2×200 mL). The product was dried in air for 1 day to a constant weight to give an off-white solid (205.8, yield: 97%). M.p. 98-100° C. (dec.) In a 4-litter bottle equipped with a mechanical stirrer maintained below 50° C. by adding ice with stirring the mixture was stirred for another 30 minutes in an ice-water bath The mixture was filtered washed with aqueous trichloroacetic acid (2%, 5×200 mL) and hexanes (or heptane) (2×200 mL) The product was dried in air for 1 day to a constant weight to give an off-white solid (205.8, yield: 97%)

反応条件: temp:0.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: In a 4-litter bottle equipped with a mechanical stirrer, sodium hydroxide (80 g, 2 mol) was dissolved in water (500 mL) and the solution was cooled to 0° C. (ice-water bath). THF (200 mL), methylamine (40% in water, 170 mL, 2 mol) and carbon disulfide (120 mL, 2 mol) were added and the mixture as stirred at 0° C. for 30 minutes. Crushed ice (1.5 kg) was added, followed by glacial acetic acid (300 mL). Hydrogen peroxide (30%, 100 mL, 1 mol) was added dropwise over 10 minutes with temperature maintained below 50° C. by adding ice with stirring. Hexanes (or heptane) (800 mL) was added and the mixture was stirred for another 30 minutes in an ice-water bath. The mixture was filtered and washed with aqueous trichloroacetic acid (2%, 5×200 mL) and hexanes (or heptane) (2×200 mL). The product was dried in air for 1 day to a constant weight to give an off-white solid (205.8, yield: 97%). M.p. 98-100° C. (dec.) In a 4-litter bottle equipped with a mechanical stirrer maintained below 50° C. by adding ice with stirring the mixture was stirred for another 30 minutes in an ice-water bath The mixture was filtered washed with aqueous trichloroacetic acid (2%, 5×200 mL) and hexanes (or heptane) (2×200 mL) The product was dried in air for 1 day to a constant weight to give an off-white solid (205.8, yield: 97%)

反応条件: temp:0.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: In a 4-litter bottle equipped with a mechanical stirrer, sodium hydroxide (80 g, 2 mol) was dissolved in water (500 mL) and the solution was cooled to 0° C. (ice-water bath). THF (200 mL), methylamine (40% in water, 170 mL, 2 mol) and carbon disulfide (120 mL, 2 mol) were added and the mixture as stirred at 0° C. for 30 minutes. Crushed ice (1.5 kg) was added, followed by glacial acetic acid (300 mL). Hydrogen peroxide (30%, 100 mL, 1 mol) was added dropwise over 10 minutes with temperature maintained below 50° C. by adding ice with stirring. Hexanes (or heptane) (800 mL) was added and the mixture was stirred for another 30 minutes in an ice-water bath. The mixture was filtered and washed with aqueous trichloroacetic acid (2%, 5×200 mL) and hexanes (or heptane) (2×200 mL). The product was dried in air for 1 day to a constant weight to give an off-white solid (205.8, yield: 97%). M.p. 98-100° C. (dec.) In a 4-litter bottle equipped with a mechanical stirrer maintained below 50° C. by adding ice with stirring the mixture was stirred for another 30 minutes in an ice-water bath The mixture was filtered washed with aqueous trichloroacetic acid (2%, 5×200 mL) and hexanes (or heptane) (2×200 mL) The product was dried in air for 1 day to a constant weight to give an off-white solid (205.8, yield: 97%)

反応条件: temp:0.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: In a 4-litter bottle equipped with a mechanical stirrer, sodium hydroxide (80 g, 2 mol) was dissolved in water (500 mL) and the solution was cooled to 0° C. (ice-water bath). THF (200 mL), methylamine (40% in water, 170 mL, 2 mol) and carbon disulfide (120 mL, 2 mol) were added and the mixture as stirred at 0° C. for 30 minutes. Crushed ice (1.5 kg) was added, followed by glacial acetic acid (300 mL). Hydrogen peroxide (30%, 100 mL, 1 mol) was added dropwise over 10 minutes with temperature maintained below 50° C. by adding ice with stirring. Hexanes (or heptane) (800 mL) was added and the mixture was stirred for another 30 minutes in an ice-water bath. The mixture was filtered and washed with aqueous trichloroacetic acid (2%, 5×200 mL) and hexanes (or heptane) (2×200 mL). The product was dried in air for 1 day to a constant weight to give an off-white solid (205.8, yield: 97%). M.p. 98-100° C. (dec.) In a 4-litter bottle equipped with a mechanical stirrer maintained below 50° C. by adding ice with stirring the mixture was stirred for another 30 minutes in an ice-water bath The mixture was filtered washed with aqueous trichloroacetic acid (2%, 5×200 mL) and hexanes (or heptane) (2×200 mL) The product was dried in air for 1 day to a constant weight to give an off-white solid (205.8, yield: 97%)