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Trimethylaluminum → HCID 178456261、化合物
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Trimethylaluminum | HCID 16682925 | — |
| 反応物 | Ethyl ether methylene chloride | HCID 21881112 | — |
| 反応物 | Ethyl 4-(4-allyl-1,4-diazepan-1-yl)benzoate | HCID 66589947 | — |
| 反応物 | HCID 178489815 | HCID 178489815 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | HCID 178456261 | HCID 178456261 | 14.5% |
反応手順
N-[5-[2-(3,5-dimethoxyphenyl)ethyl]-2H-pyrazol-3-yl]-4-(4-prop-2-enyl-1,4-diazepan-1-yl)benzamide was prepared using the same procedure as for Example 159, but starting from ethyl 4-(4-allyl-1,4-diazepan-1-yl)benzoate (0.288 g, 1 mmol, 5-[2-(3,5-dimethoxyphenyl)ethyl]-2H-pyrazol-3-amine (0.247 g, 1 mmol) and a 2M solution of trimethylaluminium (1.250 mL, 2.50 mmol) in toluene. The crude product was purified by preparative HPLC, using decreasingly polar mixtures of water (containing 1% NH3) and MeCN as eluents. Fractions containing the desired compound were evaporated to dryness to afford a gum, which solidified on trituration with DCM/Ether to afford the title compound (0.071 g, 14.50%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07737149B2 |
| 出典データセット | uspto-grants-2010_06 |
| ORD ID | ord-9eb3daab9187492aa4087e7b7789c753 |
| 出典メモ | uspto-grants-2010_06 |