関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 4-Fluorobenzonitrile | HCID 14517 | — |
| 反応物 | tert-Butyl (2S)-2-methylpiperazine-1-carboxylate | HCID 10081508 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | (S)-tert-butyl 4-(4-cyanophenyl)-2-methylpiperazine-1-carboxylate | HCID 58324511 | 30% |
反応手順
(S)-tert-butyl 2-methylpiperazine-1-carboxylate (1 g, 4.99 mmol), 4-fluorobenzonitrile (0.605 g, 4.99 mmol), and K2CO3 (0.897 g, 6.49 mmol) were combined into a vial equipped with a stir bar. The reaction was heated to 110° C. for 48 h. Cooled to RT, diluted with EA and filtered. Concentrated to a clear oil and purified on silica gel (80 g, 10-20% EA in Hex) to give a clear oil (450 mg, 30% yield) which became a crystalline solid upon sitting. [M+H] calc'd for C17H23N3O2, 301; found, 301.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US08124606B2 |
|---|
| 出典データセット | uspto-grants-2012_02 |
|---|
| ORD ID | ord-f4238f6091e74e8986411067b35f7fa6 |
|---|
| 出典メモ | uspto-grants-2012_02 |
|---|
