関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrazine | HCID 9321 | — |
| 反応物 | Ammonium Hydroxide | HCID 14923 | — |
| 反応物 | Dichloromethane methanol | HCID 21226129 | — |
| 反応物 | Methyl 3-(2-fluorophenyl)-2-(2-(isopropylamino)benzo[d]thiazol-6-yl)-3-oxopropanoate | HCID 57527151 | — |
| 溶媒 | Acetic Acid | HCID 176 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | HCID 178456807 | HCID 178456807 | 27% |
反応手順
To a solution of methyl 3-(2-fluorophenyl)-2-(2-(isopropylamino)benzo[d]thiazol-6-yl)-3-oxopropanoate(63% purity, 0.260 g) in glacial AcOH (4 mL) and EtOH (2 mL) was added anhydrous hydrazine (0.18 mL, 5.73 mmol) at 0° C. The resulting mixture was heated at 85° C. for 4 hr. After it cooled to rt, the mixture was diluted with water (40 mL), basified with concentrated ammonium hydroxide to pH 8, and extracted with AcOEt (3×30 mL). The combined extract was washed with brine and dried over anhydrous MgSO4. The title compound (55.0 mg, 27% yield over two steps) was isolated by ISCO (8% MeOH/CH2Cl2). (M+H)+=369.21.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07994337B2 |
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| 出典データセット | uspto-grants-2011_08 |
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| ORD ID | ord-d37f9aed406d4ca99b34109e48de668e |
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| 出典メモ | uspto-grants-2011_08 |
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