참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | 1,2-Dichloroethane | HCID 11 | — |
| 반응물 | Sodium Hydroxide | HCID 14798 | — |
| 반응물 | 1-Hydroxybenzotriazole | HCID 75771 | — |
| 반응물 | Methyl 2-(2-(pyrrolidin-1-yl)ethoxy)benzoate | HCID 59733402 | — |
| 반응물 | HCID 178508056 | HCID 178508056 | — |
| 용매 | Dimethyl Sulfoxide | HCID 679 | — |
| 용매 | Water | HCID 962 | — |
| 생성물 | HCID 178522448 | HCID 178522448 | 14% |
반응 단계
2-(2-Pyrrolidin-1-yl-ethoxy)-benzoic acid methyl ester (0.104 g, 0.42 mmol) was treated with 2 M aqueous NaOH (20 ml) and water (20 ml). The reaction mixture was stirred at room temperature for 20 hours, then reduced in vacuo and azeotroped with toluene (3×5 ml). Water (50 ml) was added and the mixture taken to pH 5 using 1M aqueous HCl. The resulting solution was reduced in vacuo and azeotroped with toluene (3×5 ml) to give a white solid, which was combined with 4-amino-1H-pyrazole-3-carboxylic acid (4-fluoro-phenyl)-amide (Example 2B) (0.055 g, 0.25 mmol), EDC (0.058 g, 0.3 mmol) and HOBt (0.041 g, 0.3 mmol) and stirred at room temperature in DMSO (3 ml) for 20 hours. The reaction mixture was poured into water (30 ml) and the resultant solid was collected by filtration and dried in a vacuum oven to give the title compound as a grey solid (0.015 g, 14%). (LC/MS: Rt 2.18, [MH]+ 438.06).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 특허 번호 | US07745638B2 |
|---|
| 출처 데이터셋 | uspto-grants-2010_06 |
|---|
| ORD ID | ord-f7ed526206b0425482851bd0b48cd898 |
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| 출처 메모 | uspto-grants-2010_06 |
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