関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | Chlorosulfamic acid | HCID 24499 | — |
| 反応物 | 2-(2-Chlorophenoxy)ethanol | HCID 84933 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 生成物 | Sulfamic acid 2-(2-chlorophenoxy)ethyl ester | HCID 19108707 | 58% |
反応手順
The title compound was obtained using the following procedure: The sulfamoyl chloride solution prepared in (a) was reacted as in Example 4 with 17.3 g (0.100 mole) of 2-(2-chlorophenoxy)ethanol and 40.4 g (0.400 mole) of triethylamine in 100 ml of acetonitrile followed by extraction, washing and concentration procedures of Example 4 through the first evaporation. The viscous, oily residue was partitioned between 500 ml of water and 500 ml of ethyl ether. The organic layer was washed with four 300 ml portions of water (pH of wash finally neutral to pH paper), dried over magnesium sulfate and the solvent evaporated under reduced pressure to give a white solid. The solid was recrystallized from ethyl ether-petroleum ether (bp 30°-60° C.) to give 14.5 g (58%) of title compound as white solid, mp 84.5°-86° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05025031 |
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| 出典データセット | uspto-grants-1991_06 |
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| ORD ID | ord-1fccb8bc43b44448a43a5370cffb4272 |
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| 出典メモ | uspto-grants-1991_06 |
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