関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Methanol | HCID 887 | — |
| 反応物 | Thionyl Chloride | HCID 24386 | — |
| 反応物 | 4-(Aminomethyl)Benzoic Acid | HCID 65526 | — |
| 生成物 | Methyl 4-(aminomethyl)benzoate hydrochloride | HCID 2729253 | — |
反応手順
3.3 cm3 of thionyl chloride are added over 10 minutes to 30 cm3 of methanol cooled to a temperature in the region of -30° C. Stirring is maintained for 30 minutes at a temperature in the region of -23° C. and then 4.7 g of 4-aminomethylbenzoic acid are added. The mixture is left to return to a temperature in the region of 20° C. over 1 hour. The mixture is treated with 15 cm3 of methanol and stirring is maintained for 15 hours at a temperature in the region of 20° C. The solid is separated by filtration, rinsed with a total of 90 cm3 of methanol and then with a total of 150 cm3 of diethyl ether. The solid is dried under reduced pressure (13.5 Pa) at a temperature in the region of 20° C. 3.2 g of methyl 4-aminomethylbenzoate hydrochloride are thus obtained in the form of a white solid melting at a temperature in the region of 270° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05468888 |
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| 出典データセット | uspto-grants-1995_11 |
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| ORD ID | ord-c1f2689f3d6e404dbe56ad3975977d0d |
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| 出典メモ | uspto-grants-1995_11 |
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