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Azobisisobutyronitrile → 5-(Bromomethyl)thiophene-2-carbonitrile
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Azobisisobutyronitrile | HCID 6547 | — |
| 反応物 | N-bromobutanimide | HCID 67184 | — |
| 反応物 | 5-Methylthiophene-2-carbonitrile | HCID 312733 | — |
| 反応物 | Nbs aibn | HCID 86630000 | — |
| 生成物 | 5-(Bromomethyl)thiophene-2-carbonitrile | HCID 10560016 | — |
反応手順
1.69 kg (9.51 moles) of NBS and 156 g (0.95 moles) of AIBN were well mixed and placed in a vinyl wrapper (at this time, the previous reaction was regarded to be proceeded to 100%). The benzene solution of Example 2 was heated. The NBS-AIBN mixture was portionwise added to the heated solution at 73° C. for 40 minutes. The solution was refluxed for 1.5 hours after the addition was done. After confirming completion of the reaction by HPLC, the solution was cooled to room temperature. The reaction solution was washed with [1 L of H2O+4 L of 5% NaHCO3], and then [2 L of H2O+1 L of 5% NaCl].
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07015337B2 |
| 出典データセット | uspto-grants-2006_03 |
| ORD ID | ord-2f748aa9f05543a6be1386a4cd7d79dc |
| 出典メモ | uspto-grants-2006_03 |