関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Dimethylformamide | HCID 6228 | — |
| 反応物 | Sodium Carbonate | HCID 10340 | — |
| 反応物 | N-Methyl-N-naphthylmethylamine | HCID 84474 | — |
| 反応物 | Benzene, 1-(chloromethyl)-4-(1,1-dimethylethyl)- | HCID 88198 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | Butenafine Hydrochloride | HCID 443867 | — |
反応手順
A mixture of 3.43 g of N-methyl-naphthylmethylamine, 3.65 g of 4-tert-butylbenzyl chloride, 2.33 g of anhydrous sodium carbonate and 20 ml of dimethyl formamide was stirred at 50° C. for 16 hours. The reaction mixture was poured into water and extracted with benzene, and the benzene solution was washed with water. After distilling away benzene, 3 ml of concentrated hydrochloric acid was added at cooling. An excess of hydrochloric acid was removed under reduced pressure and a suitable amount of acetone was added. White crystal (5.9 g) was precipitated and was filtered. N-(4-tertbutylbenzyl)-N-methyl-lnaphthylmethylamine hydrochloride of white plate crystal (Compound of Example 1) was obtained by recrystallization from acetone/ethanol. Melting point: 210° to 212° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | USRE034770 |
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| 出典データセット | uspto-grants-1994_11 |
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| ORD ID | ord-f2a995087ddf40cdb73c9411ada2fdaa |
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| 出典メモ | uspto-grants-1994_11 |
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