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2-Bromo-6-chlorobenzo[d]thiazole → Methyl (4-(6-chloro-2-benzothiazolyl)amino-3-chlorophenyl)acetate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 2-Bromo-6-chlorobenzo[d]thiazole | HCID 11499762 | — |
| 反応物 | Methyl 2-(4-amino-3-chlorophenyl)acetate | HCID 13616273 | — |
| 反応物 | Pyridinium.p-toluenesulfonate | HCID 22033616 | — |
| 溶媒 | O-Xylene | HCID 7237 | — |
| 生成物 | Methyl (4-(6-chloro-2-benzothiazolyl)amino-3-chlorophenyl)acetate | HCID 58778710 | 24.1% |
反応手順
In xylene (10 ml), 2-bromo-6-chlorobenzothiazole (760 mg, 3.06 mmol), methyl 4-amino-3-chlorophenylacetate (610 mg, 3.06 mmol), and pyridinium•p-toluenesulfonate (PPTS) (230 mg, 0.92 mmol) were heated under reflux for 1 hour. After cooling, the reaction mixture was distilled under reduced pressure to remove the solvent. The residue was purified by chromatography on a silica gel column, whereby from n-hexane/ethyl acetate (6:1, v/v) eluate fractions, methyl (4-(6-chloro-2-benzothiazolyl)amino-3-chlorophenyl)acetate (271 mg, 24%) was obtained as a pale yellow solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07157487B2 |
| 出典データセット | uspto-grants-2007_01 |
| ORD ID | ord-132831e55ece48d098a49cee79ce59c0 |
| 出典メモ | uspto-grants-2007_01 |