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Thiosemicarbazide → 4-(3,4-Dichlorophenyl)-2-hydrazinylthiazole
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Thiosemicarbazide | HCID 2723789 | — |
| 反応物 | 3,4-Dichlorophenylacetyl bromide | HCID 86642370 | — |
| 溶媒 | 1,4-Dioxane | HCID 31275 | — |
| 生成物 | 4-(3,4-Dichlorophenyl)-2-hydrazinylthiazole | HCID 7174071 | — |
反応手順
A solution of a thiosemicarbazide (10 mmol, 0.91 g) and 3,4-dichlorophenylacetyl bromide (10 mmol, 2.68 g) in dioxane (20 mL) was stirred at room temperature for 16 h. The precipitate of hydrobromide salt was filtered and washed with dioxane (3×10 mL) basified with 2N Na2CO3 (20 mL). The product was filtered, washed with water and dried (2.08 g, 80%). The product was generally satisfactory for further reaction. 1H NMR (400 MHz) δ 8.67 (s, 1H, NH), 8.00 (d, J=1.6 Hz, 1H), 7.76 (dd, J=1.6 Hz, J=8.4 Hz, 1H), 7.60 (d, J=8.4 Hz, 1H), 7.31 (s), 1H MS+(APCI), 259.68, (M+1; calcd 258.97 (M+)
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08257931B2 |
| 出典データセット | uspto-grants-2012_09 |
| ORD ID | ord-5cd2ac8b052e4ca09fd45ebe0d67200c |
| 出典メモ | uspto-grants-2012_09 |