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Triethylamine → HCID 66750860、化合物
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | 1-Ethyl-3-(3'-dimethylaminopropyl)carbodiimide | HCID 15908 | — |
| 反応物 | 1-Hydroxybenzotriazole | HCID 75771 | — |
| 反応物 | Sodium Bicarbonate | HCID 516892 | — |
| 反応物 | Methyl 4-(2-aminoethyl)benzoate hydrochloride | HCID 13078671 | — |
| 反応物 | HCID 66750854 | HCID 66750854 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | HCID 66750860 | HCID 66750860 | 71.5% |
反応手順
A mixture of 2-[4-(2-tert-butylphenyl)piperazin-1-yl]-2-oxoacetic acid (Example 44, 1.0 g, 3.44 mmol), methyl 4-(2-aminoethyl)benzoate hydrochloride (0.83 g, 4.13 mmol), triethylamine (0.72 mL, 5.16 mmol), EDCI (0.64 g, 4.13 mmol) and HOBt (0.63 g, 4.13 mmol) in N,N-dimethylformamide (10 mL) was stirred at room temperature for 16 h. The reaction mixture was poured into saturated NaHCO3 solution and extracted with ethyl acetate. The extract was washed with saturated NaHCO3 solution and brine, dried over anhydrous magnesium sulfate, filtered and concentrated under reduced pressure. The residue was purified by silica gel column chromatography (hexane/ethyl acetate 80:20 to 34:66) to give the title compound (1.11 g, 71%) as a white amorphous.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08853215B2 |
| 出典データセット | uspto-grants-2014_10 |
| ORD ID | ord-375f6e52ea0e48eca00b0610d81ad806 |
| 出典メモ | uspto-grants-2014_10 |