関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Acetic Acid | HCID 176 | — |
| 反応物 | 4-Aminobenzoic Acid | HCID 978 | — |
| 反応物 | Ammonium thiocyanate | HCID 15666 | — |
| 反応物 | Bromine | HCID 24408 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 6-Benzothiazolecarboxylic acid, 2-amino- | HCID 66740 | — |
反応手順
220 parts of the β-acetoxyethyl ester of p-aminobenzoic acid and 333 parts of ammonium thiocyanate are suspended in 1000 parts of acetic acid. The suspension is cooled to 15° C. and then a solution of 176 parts of bromine in 300 parts of acetic acid is gradually added in a period of two hours, without allowing the temperature to exceed 15° C. The mixture is stirred for an hour at 15° C. and then allowed to stand overnight and is subsequently run into 2500 parts of water containing 15 parts of 19° Be hydrochloric acid. Then it is heated to 95° C., filtered at 95° C., and the cooled filtrate is neutralised by the addition of 700 parts of sodium carbonate, filtered again, and the precipitate is washed with 2000 parts of water, drained and dried at 60° C. 215 parts of β-acetoxyethyl ester of 2-amino-benzothiazole-6-carboxylic acid, m.p. 191°-192° C, are thus obtained.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04013632 |
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| 出典データセット | uspto-grants-1977_03 |
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| ORD ID | ord-a8dd541049d146c79c9afc2306d313b7 |
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| 出典メモ | uspto-grants-1977_03 |
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