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Benzene → HCID 15291091、化合物
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Benzene | HCID 241 | — |
| 反応物 | 18-Crown-6 | HCID 28557 | — |
| 反応物 | Sodium Azide | HCID 33557 | — |
| 反応物 | 2-(Chloromethyl)-4-isopropyl-6-methoxybenzo[D]isothiazol-3(2H)-one 1,1-dioxide | HCID 9995173 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | HCID 15291091 | HCID 15291091 | 26% |
反応手順
A solution of 18-crown-6 ether (0.60 g) and benzene (60 mL) was heated under reflux with a water separator for 1 hour, then cooled to room temperature. 2-Chloromethyl-4-isopropyl-6-methoxysaccharin (3.03 g) and sodium azide (0.65 g) were added, and the mixture was stirred for a week at room temperature, then chromatographed on a column of silica gel (silica gel 60, 83 g) using benzene as eluant. The fractions containing the product, which were identified by thin layer chromatography, were combined and concentrated affording 2-azidomethyl-4-isopropyl-6-methoxysaccharin as a solution in benzene (250 mL).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05464852 |
| 出典データセット | uspto-grants-1995_11 |
| ORD ID | ord-1d4838076b604dfe911e87f95da97d89 |
| 出典メモ | uspto-grants-1995_11 |