関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Glycine | HCID 750 | — |
| 反応物 | Sodium Chloride | HCID 5234 | — |
| 反応物 | Benzoyl chloride, 3-nitro- | HCID 8495 | — |
| 反応物 | Potassium Hydroxide | HCID 14797 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 生成物 | Glycine, N-(3-nitrobenzoyl)- | HCID 94858 | 90% |
反応手順
Glycine (20 g, 266 mmol) was added to water (200 mL), followed by potassium hydroxide (20 g, 357 mmol) and cooled to 0° C. in an ice bath. To this solution was added 3-nitrobenzoyl chloride (20 g, 108 mmol) in acetonitrile (20 mL) drop-wise over a 10 minute period. After the reaction was complete (3-4 hours) concentrated hydrochloric acid was added until pH=2 followed by saturated aqueous NaCl (75 mL). The product was filtered, washed with water and air dried (22 g, 90% yield). 1H-NMR (d6 -DMSO) δ 3.92 (d, 2H, J=6.1), 7.9 (t, 1H, J=7.9), 8.3 (t, 1H, J=5.6), 8.35 (m, 2H), 8.69 (s, 1H), 9.25 (t, 1H, J=7.2 Hz).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US06028223 |
|---|
| 出典データセット | uspto-grants-2000_02 |
|---|
| ORD ID | ord-6437b511a083456b9ca417d762df1447 |
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| 出典メモ | uspto-grants-2000_02 |
|---|
