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Ethyl Acetoacetate → HCID 178472848、化合物
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Ethyl Acetoacetate | HCID 8868 | — |
| 反応物 | Sodium Bicarbonate | HCID 516892 | — |
| 反応物 | Sodium Nitrite | HCID 23668193 | — |
| 反応物 | 3'-Amino-2'-methoxy-[1,1'-biphenyl]-3-carboxylic acid | HCID 57483786 | — |
| 溶媒 | Hydrochloric Acid | HCID 313 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | HCID 178472848 | HCID 178472848 | — |
反応手順
To a solution of 3′-amino-2′-methoxybiphenyl-3-carboxylic acid (5 g) prepared as in Example 6, in hydrochloric acid (8.5 mL) and methanol (90 mL) was added a solution of sodium nitrite (1.41 g in 400 mL of water) at about 0° C. to about 5° C. under stirring. The reaction mixture was stirred for about 15 minutes at about 5° C. Then ethyl acetoacetate (2.7 g) was added and the reaction mixture was stirred for about 15 minutes at about 0° C. to about 5° C. Solid sodium bicarbonate (15 g) and ethanol (30 mL) was added and the reaction mixture was allowed to warm to about room temperature and stirred for about 2 hours. The mixture was filtered, washed with water (50 mL) and dried under vacuum at about 35° C. to about 40° C. for about 6 hours.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US09440927B2 |
| 出典データセット | uspto-grants-2016_09 |
| ORD ID | ord-122bb4bae9464a4a9d01a270231344af |
| 出典メモ | uspto-grants-2016_09 |