関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Triethyl ethane-1,1,2-tricarboxylate | HCID 81961 | — |
| 反応物 | Sodium Methoxide | HCID 10942334 | — |
| 反応物 | 2-(4-Nitrophenyl)ethanimidamide hydrochloride | HCID 46318421 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | HCID 178499608 | HCID 178499608 | — |
反応手順
A 250 mL round bottom flask was charged with 2-(4-nitrophenyl)ethanimidamide hydrochloride (approximately 6.47 g, 30.0 mmol, 48% purity), triethyl ethane-1,1,2-tricarboxylate (7.60 mL, 33.0 mmol) and methanol (43 mL). To this solution was added a 25% sodium methoxide solution in methanol (24.0 mL, 105.2 mmol) immediately resulting in a dark purple thick suspension. After stirring for three hours under reflux the dark purple mixture was cooled to 0° C. using an ice bath and carefully treated with 30 mL water. This mixture was slowly treated with 35 mL 6N hydrochloric acid giving a pale green suspension. The suspension was stirred for additional 30 minutes, filtered and the obtained fawn solid was washed with 100 mL water. The product was dried in a desiccator under vacuum for two days. The crude product was used without purification in the next step.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08541419B2 |
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| 出典データセット | uspto-grants-2013_09 |
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| ORD ID | ord-896753e013a64ab8ab5ba568d4ebf1c3 |
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| 出典メモ | uspto-grants-2013_09 |
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