関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Toluene | HCID 1140 | — |
| 反応物 | Phosgene | HCID 6371 | — |
| 反応物 | Sodium Bicarbonate | HCID 516892 | — |
| 反応物 | 4-Amino-5,6,7,8-tetrahydronaphthalene-1-carbonitrile, hydrochloride salt | HCID 131726977 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 4-Isocyanato-5,6,7,8-tetrahydronaphthalene-1-carbonitrile | HCID 59754304 | 99.8% |
反応手順
To a stirring suspension of compound 2D (0.10 g, 0.48 mmol) and NaHCO3 (0.404 g, 4.80 mmol) in CH2Cl2 (4 mL) cooled to 0° C. was rapidly added a solution of phosgene (20%) in toluene (0.95 mL, 4.32 mmol). After addition, the mixture was stirred at rt for 2 h, then filtered to remove the solid. The filtrate was concentrated under reduced pressure, the resulting solid residue dried under vacuum for 1 h to afford compound 2E (95 mg) as a light yellow solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US07772267B2 |
|---|
| 出典データセット | uspto-grants-2010_08 |
|---|
| ORD ID | ord-d93fd10229394289bffabb38e613fd6d |
|---|
| 出典メモ | uspto-grants-2010_08 |
|---|
