関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Benzene, 4-bromo-1,2-dimethoxy- | HCID 76114 | — |
| 反応物 | (R)-1-Boc-2-isopropylpiperazine | HCID 24820392 | — |
| 試薬 | Potassium tert-butoxide | HCID 23665647 | — |
| 触媒 | Tris(1,1-dimethylethyl)phosphine | HCID 83681 | — |
| 触媒 | Bis(tri-tert-butylphosphine)palladium(0) | HCID 2734558 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | tert-butyl (2R)-4-(3,4-dimethoxyphenyl)-2-propan-2-ylpiperazine-1-carboxylate | HCID 69098812 | 90.52% |
反応手順
22-Apr-09 09:56:23 +0100 4-bromo-1,2-dimethoxybenzene (0.068 mL, 0.46 mmol), (R)-tert-butyl 2-isopropylpiperazine-1-carboxylate (126 mg, 0.55 mmol) and BIS(TRI-T- BUTYLPHOSPHINE)PALLADIUM(0) (23.54 mg, 0.05 mmol) and potassium 2-methylpropan-2-olate (76 mg, 0.64 mmol) were suspended in THF (5 mL) and sealed into a microwave tube. The reaction was heated to 150 °C for 10 minutes in the microwave reactor and cooled to RT. LC-MS shows no starting material. The reaction mixture was filtered and the crude product was purified by flash silica chromatography, elution gradient 0 to 20% EtOAc in isohexane. Pure fractions were evaporated to dryness to afford (R)-tert-butyl 4-(3,4-dimethoxyphenyl)-2-isopropylpiperazine-1-carboxylate (152 mg, 91 %) as a yellow gum.
情報源と証拠
| 出典データセット | 750 AstraZeneca ELN dataset |
|---|
| ORD ID | ord-dcac8bcfa5124a8baee8e28e5e992678 |
|---|
| 出典メモ | 750 AstraZeneca ELN dataset |
|---|
