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Hydrochloric Acid → HCID 178419015、化合物
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Triethylamine hydrobromide | HCID 12493 | — |
| 反応物 | Sodium Azide | HCID 33557 | — |
| 反応物 | 4-tert-Butylbenzonitrile | HCID 77883 | — |
| 反応物 | Lithium Chloride | HCID 433294 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | HCID 178419015 | HCID 178419015 | 70.7% |
反応手順
In a 250 ml round-bottomed flask fitted with reflux condenser, 4.9 g of p-t-butylbenzonitrile, 3.82 g of lithium chloride and 5.85 g of sodium azide and 8.2 g of triethylammonium bromide in 100 ml of DMF are heated at 120° C. for 8 hours. After cooling to room temperature, 100 ml of water are added and the mixture is admicxed in an ice bath with dilute hydrochloric acid until no further solid precipitates. The precipitate is filtered off with suction, washed with water and dried. Recrystallization from ethanol/water gives 4.4 g of colorless crystals.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07088757B1 |
| 出典データセット | uspto-grants-2006_08 |
| ORD ID | ord-54b352adf61040b1b1cb278b819ac59a |
| 出典メモ | uspto-grants-2006_08 |