関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Methanol | HCID 887 | — |
| 反応物 | 3-Amino-4-methoxybenzoic acid | HCID 17823 | — |
| 反応物 | Thionyl Chloride | HCID 24386 | — |
| 生成物 | Methyl 3-amino-4-methoxybenzoate hydrochloride | HCID 69298967 | 96% |
反応手順
Thionyl chloride (8.7 mL) is added dropwise to methanol (90 mL) at −30° C. under argon gas atmosphere over a period of 15 minutes and a mixture is stirred at −20° C. for 30 minutes. To the mixture is added 3-amino-4-methoxybenzoic acid (5.0 g) and the solution is stirred at the same temperature for 15 minutes and at room temperature for 3 days. The reaction mixture is concentrated in vacuo and the resultant crystals are washed with methanol/ether to give methyl 3-amino-4-methoxybenzoate hydrochloride (6.25 g, yield; 96%) as colorless crystals. M.p. 213-215° C., MS (APCI) m/z: 182 [M+H]+
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07384952B2 |
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| 出典データセット | uspto-grants-2008_06 |
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| ORD ID | ord-9e874705f6394bc8806f3d6634579f66 |
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| 出典メモ | uspto-grants-2008_06 |
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