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2,5-Dihydroxybenzoic acid → HCID 178426858、化合物
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 2,5-Dihydroxybenzoic acid | HCID 3469 | — |
| 反応物 | Tolterodine | HCID 443879 | — |
| 溶媒 | Acetone | HCID 180 | — |
| 生成物 | HCID 178426858 | HCID 178426858 | 42.5% |
反応手順
3.25 g of tolterodine dissolved in 50 mL of acetone was mixed at room temperature (25° C.) with 4.80 g of gentisic acid, which was suspended in 50 mL of acetone, and then stirred. Acetone in the above mixture was removed by nitrogen reflux apparatus, and when about 10 20 mL of acetone was removed there started to appear a solid precipitate. After stirring the mixture at room temperature (25° C.) for 1 hour, the solid precipitate was filtered and then washed with hexane. The resultant was dried at room temperature (25° C.) for 24 hours and 2.04 g (theoretical yield: 42.5%) of the final product in white solid was obtained.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08367726B2 |
| 出典データセット | uspto-grants-2013_02 |
| ORD ID | ord-e381d6cfd33c4dde97db0152e45ecbce |
| 出典メモ | uspto-grants-2013_02 |