関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Glycine | HCID 750 | — |
| 反応物 | Sodium Glycinate | HCID 4684308 | — |
| 反応物 | Sodium Methoxide | HCID 10942334 | — |
| 反応物 | 3-Isoquinolinecarboxylic acid, 4-hydroxy-1-methyl-7-phenoxy-, methyl ester | HCID 71244895 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | FG 4592 | HCID 11256664 | 86.1% |
反応手順
A pressure flask was charged with 3e (30.92 g), glycine (22.52 g), methanol (155 mL), sodium methoxide solution (64.81 g) and sealed (as an alternative, sodium glycinate was used in place of glycine and sodium methoxide). The reaction was heated to about 110° C. until reaction was complete. The mixture was cooled, filtered, washed with methanol, dried under vacuum, dissolved in water and washed with ethyl acetate. The ethyl acetate was removed and to the resulting aqueous layer an acetic acid (18.0 g) solution was added. The suspension was stirred at room temperature, filtered, and the solid washed with water (3×30 mL), cold acetone (5-10° C., 2×20 mL), and dried under vacuum to obtain 2-(4-hydroxy-1-methyl-7-phenoxyisoquinoline-3-carboxamido)acetic acid (Yield: 86.1%, HPLC: 99.8%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US09340511B2 |
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| 出典データセット | uspto-grants-2016_05 |
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| ORD ID | ord-07705635484f42dcbae9b04aa3cbbdd9 |
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| 出典メモ | uspto-grants-2016_05 |
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