関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Salicylaldehyde | HCID 6998 | — |
| 反応物 | 1,3-Benzenedimethanamine | HCID 15133 | — |
| 触媒 | Nickel | HCID 935 | — |
| 溶媒 | Isopropanol | HCID 3776 | — |
| 生成物 | N,N'-Bis-(2-hydroxybenzyl)-m-xylylenediamine | HCID 22756078 | 41.8% |
反応手順
34.4 g of a bisazomethine prepared from 2 mols of salicylaldehyde and 1 mol of m-xylylenediamine and having a melting point of 61°-63° C. are hydrogenated for 7 hours in 170 ml of isopropanol in an autoclave in the presence of 4 g of Raney nickel at 85° C. and under a pressure of 60 atmospheres. The catalyst is filtered off and the filtrate is concentrated in a rotary evaporator to give 35.8 g of crude product. 25.7 g are recrystallised from 77 ml of isopropanol and the bulk of the product separates out on cooling in a refrigerator. The precipitate is collected by filtration, washed off with cold isopropanol and dried in vacuo at 40° C., affording 11.0 g (41.8% of theory) of N,N'-bis-(2-hydroxybenzyl)-m-xylylenediamine with a melting point of 67°-68° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04129556 |
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| 出典データセット | uspto-grants-1978_12 |
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| ORD ID | ord-3cf7519bbe4349b79ea103fe0719360e |
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| 出典メモ | uspto-grants-1978_12 |
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