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Chloroform → HCID 178526560、化合物
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Chloroform | HCID 6212 | — |
| 反応物 | 4-Nitroindazole | HCID 18057 | — |
| 反応物 | Bromine | HCID 24408 | — |
| 反応物 | Sodium Acetate | HCID 517045 | — |
| 溶媒 | Acetic Acid | HCID 176 | — |
| 生成物 | HCID 178526560 | HCID 178526560 | 86.9% |
反応手順
Sodium acetate (52.8 g, 644 mmol) and 4-nitro-1H-indazole (100 g, 613 mmol) were mixed with acetic acid (1000 mL) and chloroform (1000 mL) in a 5 L 4-neck flask with mechanical stirring. A solution of bromine (103 g, 644 mmol) in acetic acid (120 mL) was added over approximately 3.5 hours, while keeping the temperature below 21° C. After the addition was completed, the reaction mixture was stirred for an additional 2 hours. The reaction mixture was concentrated under reduced pressure. Water (2000 mL) was added to the residue. The yellow solids were collected by filtration and washed with water (3×1000 mL). The solids were air-dried on the filter and then under vacuum at 40° C. to give the desired product (129 g) as a yellow solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08841455B2 |
| 出典データセット | uspto-grants-2014_09 |
| ORD ID | ord-20188b337dbc41338ecb8a954ab12147 |
| 出典メモ | uspto-grants-2014_09 |