関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 2-(3,4,5-trimethoxyphenyl)acetyl Chloride | HCID 11032124 | — |
| 反応物 | 4-[2-(Pyrrolidin-3-yloxy)ethyl]morpholine | HCID 21333165 | — |
| 溶媒 | Benzene | HCID 241 | — |
| 生成物 | 3-(2-Morpholinoethoxy)-1-(3,4,5-trimethoxyphenylacetyl) pyrrolidine Hemihydrate | HCID 70605083 | 70% |
反応手順
Under anhydrous conditions 5.3 g. crude 3,4,5-trimethoxyphenylacetic acid chloride [equivalent to 4.5 g. (0.0184 mole) by nuclear resonance spectrum analysis] in 20 ml. dry benzene was added dropwise to a stirring mixture of 3.7 g. (0.0184 mole) of 3-(2-morpholinoethoxy)pyrrolidine and 30 g. (0.0217 mole) of potassium carbonate in 50 ml. dry benzene. The product formed rapidly and separated out as a gummy mass. After stirring 1 hr. at room temperature, chloroform was stirred into the reaction mixture to dissolve the product. The inorganic materials were removed by filtration and the filtrate concentrated at reduced pressure to give 5.3 g. crude product (70% yield). A portion (2.6 g.) of the crude product was chromatographed on magnesium silicate to give 1.6 g. of pure product.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04096331 |
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| 出典データセット | uspto-grants-1978_06 |
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| ORD ID | ord-94936033071b4c399849ffb9e69a4733 |
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| 出典メモ | uspto-grants-1978_06 |
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