関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Ammonia | HCID 222 | — |
| 反応物 | Sulfuryl chloride | HCID 24648 | — |
| 反応物 | N-p-Bromophenylthiourea | HCID 2735620 | — |
| 反応物 | Magnesium monoxide | HCID 6850729 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Chlorobenzene | HCID 7964 | — |
| 生成物 | 2-Benzothiazolamine, 6-bromo- | HCID 85149 | 49.6% |
反応手順
A solution of N-(4-bromophenyl)thiourea (16.18 g) and magnesium oxide (1.41 g) in chlorobenzene (100 mL) was heated to 50° C., and a solution of sulfuryl chloride (8.43 mL) in chlorobenzene (9 mL) was added dropwise to the solution over 1 hour or longer, followed by stirring at 50° C. overnight. The reaction mixture was returned to room temperature, and water (20 mL) was added thereto. The pH of the mixture was adjusted to about 8 by use of concentrated aqueous ammonia, and the precipitates were recovered through filtration. The obtained solid was recrystallized from 90% ethanol, to thereby yield the title compound (7.95 g).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08022075B2 |
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| 出典データセット | uspto-grants-2011_09 |
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| ORD ID | ord-b0fd9dd3609b43099be2bb67858921e4 |
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| 出典メモ | uspto-grants-2011_09 |
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