関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | 2-Methylthiophene | HCID 11126 | — |
| 反応物 | 5-Ethyl-2-hydroxybenzoyl chloride | HCID 13838820 | — |
| 溶媒 | 1,1,1,2-Tetrachloroethane | HCID 12418 | — |
| 生成物 | (2-Hydroxy-5-ethylphenyl)(5-methyl-2-thienyl)methanone | HCID 13838809 | — |
反応手順
2-Hydroxy-5-ethylbenzoyl chloride (6.08g, 0.036 mol) and 2-methylthiophene were mixed together in tetrachloroethane (20 ml), and stannic chloride (18.78g, 0.072 mol) in tetrachloroethane (20 ml) was added dropwise with stirring, the temperature of the mixture being at about 20° C. by cooling with an ice bath. The mixture was then stirred at room temperature for 3 hours and left to stand at room temperature overnight. The resulting pink solution was poured into ice and concentrated hydrochloric acid (10 to 20 ml), stirred until the ice had melted and extracted with chloroform. The chloroform extract was washed firstly with a saturated solution of sodium bicarbonate and secondly with a saturated solution of sodium chloride, was dried (over Na2SO4), filtered and evaporated to leave an oil which distilled to give the pure title product (4.36g), bp 133°-136° C./0.1 mm, nD21 1.6341.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04131682 |
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| 出典データセット | uspto-grants-1978_12 |
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| ORD ID | ord-19ca998e01694300a435df813cd3cba0 |
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| 出典メモ | uspto-grants-1978_12 |
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