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HRID 1648757作成日:2026年10月27日

Carbofuran → Carbamic acid, ((bis(2-cyanoethyl)amino)thio)methyl-, 2,3-dihydro-2,2-dimethyl-7-benzofuranyl ester

https://huagongshe.com/reaction/1648757

反応式

関与物質

役割名称HCID仕込み量
反応物CarbofuranHCID 2566—
反応物3,3'-IminodipropionitrileHCID 8149—
反応物TriethylamineHCID 8471—
反応物Sulfur dichlorideHCID 25353—
溶媒ChloroformHCID 6212—
生成物Carbamic acid, ((bis(2-cyanoethyl)amino)thio)methyl-, 2,3-dihydro-2,2-dimethyl-7-benzofuranyl esterHCID 3067958—

反応条件

温度0 °C

反応手順

A 11 g quantity (0.05 mole) of 2,3-dihydro-2,2-dimethylbenzofuran-7-yl N-methyl-carbamate was dissolved in 50 ml of chloroform, 5.2 g (0.05 mole) of sulfur dichloride was added to the solution with cooling, and 5 g (0.05 mole) of triethylamine was further added dropwise to the solution at -10° to -5° C. The mixture was stirred at 0° C. for one hour and further at room temperature for one hour. After cooling to -10° to -5° C., 6.2 g (0.05 mole) of iminodipropionitrile was added dropwise to the mixture, and 5 g (0.05 mole) of triethylamine was further added dropwise to the mixture. The resulting mixture was stirred at 0° C. for 2 hours and thereafter allowed to stand overnight at room temperature. With addition of 100 ml of chloroform, the reaction mixture was washed with 100 ml of water three times. The chloroform layer was dried and then concentrated in a vacuum to give an oily product, which was almost entirely composed of the desired product although containing small amounts of impurities. Yield: 12.2 g (65.2%).

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US04413005
出典データセットuspto-grants-1983_11
ORD IDord-5a77e36b7c9a400abd60d1dc5c031a7c
出典メモuspto-grants-1983_11