dimethylcarbamodithioic acid

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: To a solution of 4.51 g. (0.02 mole) of 5-chloro-4-methyl-2-phenyl-4-isothiazolin-3-one in 30 ml of warm ethanol was added a solution of 3.58 g. (0.02 mole) of N,N-dimethyldithiocarbamic acid, sodium salt dihydrate in 20 ml of ethanol followed by 0.1 g. of sodium iodide. The mixture was stirred several hours, cooled and filtered. The solid was triturated with water and dried to give 5.3 g. (88%) of the named product, mp 158°-160°. cooled filtered The solid was triturated with water dried to give 5.3 g

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 mixture of 4-chloro-1-(chloromethyl)-2-(p-chlorophenyl)-5-(trifluoromethyl)pyrrole-3-carbonitrile (0.7 g, 0.002 mol) and dimethyldithiocarbamic acid, sodium salt (0.57 g, 0.004 mol) in dimethyl formamide is heated at 50°-55° for 30 minutes, cooled to room temperature and poured into water. The resultant mixture is extracted with ethyl acetate. The combined extracts are washed with a saturated sodium chloride solution, dried (MgSO4) and concentrated in vacuo to give an orange oil residue. The residue is mixed with hot hexane, cooled and filtered to give an orange solid filtercake. Recrystallization of the solid from isopropanol gives the title product as a tan crystaline solid, 0.7 g (80% yield), mp 129°-131° C. is heated at 50°-55° for 30 minutes The resultant mixture is extracted with ethyl acetate The combined extracts are washed with a saturated sodium chloride solution dried (MgSO4) concentrated in vacuo to give an orange oil residue cooled filtered to give an orange solid filtercake Recrystallization of the solid from isopropanol

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

実験手順: A solution of 9.5 g (0.053 mole) of N,N-dimethyldithiocarbamic acid (sodium salt dihydrate) in 25 ml of dimethyl sulfoxide is added dropwise at 20° C. in the course of 1 hour to a solution of 18 g (0.052 mole) of 3,5-dinitro-4-[2-methoxyethylamino]-2-chlorobenzotrifluoride in 160 ml of dimethyl sulfoxide, and the batch is stirred for 11/2 hours at room temperature. Stirring is then continued for 3 hours at 80° C. (internal temperature). For working up, the reaction mixture is poured on ice-water and extracted three times with ether. The combined ethereal phases are washed four times with water and three times with sodium chloride solution, died over sodium sulfate, filtered, and concentrated. The residue is recrystallised from ether, affording 7-[2-methoxyethylamino]-6-nitro-4-trifluoromethyl-1,3-benzodithiol-2-one with a melting point of 96°-98° C. Stirring is then continued for 3 hours at 80° C. the reaction mixture is poured on ice-water extracted three times with ether The combined ethereal phases are washed four times with water and three times with sodium chloride solution filtered concentrated The residue is recrystallised from ether

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

実験手順: A mixture of 4-chloro-1-(chloromethyl)-2-(p-chlorophenyl)-5-(trifluoromethyl)pyrrole-3-carbonitrile (0.7 g, 0.002 mol) and dimethyldithiocarbamic acid, sodium salt (0.57 g, 0.004 mol) in dimethyl formamide is heated at 50°-55° for 30 minutes, cooled to room temperature and poured into water. The resultant mixture is extracted with ethyl acetate. The combined extracts are washed with a saturated sodium chloride solution, dried (MGSO4) and concentrated in vacuo to give an orange oil residue. The residue is mixed with hot hexane, cooled and filtered to give an orange solid filtercake. Recrystallization of the solid from isopropanol gives the title product as a tan crystaline solid, 0.7 g (80% yield), mp 129°-131° C. is heated at 50°-55° for 30 minutes The resultant mixture is extracted with ethyl acetate The combined extracts are washed with a saturated sodium chloride solution dried (MGSO4) concentrated in vacuo to give an orange oil residue cooled filtered to give an orange solid filtercake Recrystallization of the solid from isopropanol

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

実験手順: A mixture of 4-chloro-1-(chloromethyl)-2-(p-chlorophenyl)-5-(trifluoromethyl)pyrrole-3-carbonitrile (0.7 g, 0.002 mol) and dimethyldithiocarbamic acid, sodium salt (0.57 g, 0.004 mol) in dimethyl formamide is heated at 50°-55° for 30 minutes, cooled to room temperature and poured into water. The resultant mixture is extracted with ethyl acetate. The combined extracts are washed with a saturated sodium chloride give an orange oil residue. The residue is mixed with hot hexane, cooled and filtered to give an orange solid filtercake. Recrystallization of the solid from isopropanol gives the title product as a tan crystaline solid, 0.7 g (80% yield), mp 129°-131° C. is heated at 50°-55° for 30 minutes The resultant mixture is extracted with ethyl acetate The combined extracts are washed with a saturated sodium chloride give an orange oil residue cooled filtered to give an orange solid filtercake Recrystallization of the solid from isopropanol

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

実験手順: To a solution of 4.51 g. (0.02 mole) of 5-chloro-4-methyl-2-phenyl-4-isothiazolin-3-one in 30 ml of warm ethanol was added a solution of 3.58 g. (0.02 mole) of N,N-dimethyldithiocarbamic acid, sodium salt dihydrate in 20 ml of ethanol followed by 0.1 g. of sodium iodide. The mixture was stirred several hours, cooled and filtered. The solid was triturated with water and dried to give 5.3 g. (88%) of the named product, mp 158°-160°. cooled filtered The solid was triturated with water dried to give 5.3 g