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Triethylsilane → 6-(2-Bromoethyl)benzothiazolone
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Triethylsilane | HCID 12052 | — |
| 反応物 | 6-(Bromoacetyl)benzothiazolinone | HCID 131717829 | — |
| 溶媒 | Trifluoroacetic acid | HCID 6422 | — |
| 生成物 | 6-(2-Bromoethyl)benzothiazolone | HCID 69227973 | — |
反応手順
In a 500-cm3 ground-necked flask surmounted by a condenser, and placed in an oil bath, 40.8 g (0.15 mol) of 6-(bromoacetyl)benzothiazolinone are dissolved in 90 cm3 of trifluoroacetic acid with magnetic stirring and while the temperature is stabilized at 60° C. 52.7 cm3 (0.33 mol) of triethylsilane are introduced dropwise via a dropping funnel. After the addition, the heating is stopped and the mixture is then left stirring vigorously for 30 hours. The reaction medium is hydrolyzed by pouring it into ice-cold water, and the precipitate obtained is drained and washed with water until the filtrate is neutral and then with hexane. The product is dried and recrystallized in absolute ethanol.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05296477 |
| 出典データセット | uspto-grants-1994_03 |
| ORD ID | ord-730a0c86cd8e45cabbb5f4a71d7944fa |
| 出典メモ | uspto-grants-1994_03 |