関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 1,2-Dichlorobenzene | HCID 7239 | — |
| 反応物 | 1,2-Ethanediamine, 4-methylbenzenesulfonate (1:?) | HCID 225030 | — |
| 反応物 | 4-Methylthio-m-tolyloxyacetonitrile | HCID 70547184 | — |
| 反応物 | 2-((4-(Methylthio)-m-tolyloxy)methyl)-2-imidazoline | HCID 70547752 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | p-Toluenesulfonic acid | HCID 6101 | 188.2% |
反応手順
The product, 2-((4-(methylthio)-m-tolyloxy)methyl)-2-imidazoline, was prepared by heating 19.3 g of 4-methylthio-m-tolyloxyacetonitrile, 23.3 g of ethylenediamine p-toluenesulfonate and 75 ml of 1,2-dichlorobenzene substantially as described in previous examples. Upon cooling the reaction mixture, diluting with CH2Cl2 and filtering, 32.5 g of p-toluenesulfonate salt was obtained. The p-toluenesulfonate salt was then slurried in water and CH2Cl2 and then basified. The CH2Cl2 layer was separated and the aqueous layer extracted with chloroform. The extracts were combined, treated with diatomaceous earth and activated charcoal and then filtered. The filtrate was taken to dryness, which gave 13.5 g of the product, 2-((4-(methylthio)-m-tolyloxy)methyl)-2-imidazoline as a white solid, m.p. 102°-104° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04343808 |
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| 出典データセット | uspto-grants-1982_08 |
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| ORD ID | ord-9f359e437e9c4394970d53471b23e6ed |
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| 出典メモ | uspto-grants-1982_08 |
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