関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Sodium Bicarbonate | HCID 516892 | — |
| 反応物 | 4-Amino-1-cyclopropylpiperidine dihydrochloride | HCID 46735243 | — |
| 反応物 | HCID 178497356 | HCID 178497356 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | HCID 178497372 | HCID 178497372 | — |
反応手順
To a mixture of 7.53 g (35.3 mmol) 1-cyclopropyl-piperidin-4-ylamine-dihydrochloride and 32.39 g (0.386 mol) NaHCO3 in 1300 mL THF and 370 mL water was added a solution of 11.79 g (32.1 mmol) 2-trichloromethyl-1H-benzoimidazole-5-carboxylic acid methyl ester in 360 mL THF. The reaction mixture was stirred vigorously for 2 h at room temperature. The THF was evaporated. The precipitate was filtered off and treated twice with approx. 300 mL of a saturated NaHCO3-solution under ultrasonic conditions. After filtration the resulting solid was washed twice with 150 mL water and dried under vacuo at 45° C. to give pure 2-(1-cyclopropyl-piperidin-4-ylcarbamoyl)-1H-benzoimidazole-5-carboxylic methyl ester in form of a light brown crystalline material. Yield: 9.9 g
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07741341B2 |
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| 出典データセット | uspto-grants-2010_06 |
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| ORD ID | ord-ecef994be21b48268334aeabeeca3dee |
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| 出典メモ | uspto-grants-2010_06 |
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