関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Methylamine | HCID 6329 | — |
| 反応物 | Thionyl Chloride | HCID 24386 | — |
| 反応物 | 5-(3,4-Dibromobutyl)pyridine-2-carboxylic acid | HCID 216720 | — |
| 溶媒 | Chloroform | HCID 6212 | — |
| 生成物 | HCID 13298527 | HCID 13298527 | — |
反応手順
According to the same method as Example 1 with cooling 30% aqueous methylamine solution (100 ml) was added to the chloroform solution (200 ml) of acid chloride prepared from 10 g of 5-(3,4-dibromobutyl)picolinic acid and 10 ml of thionyl chloride, and stirred at 8°C for an hour. Chloroform layer which was separated, was washed with 0.3% aqueous hydrochloride solution, 5% aqueous sodium bicarbonate solution, and then water. Chloroform was evaporated in reduced pressure to yield 8.7 g of crude product as oil. To purify the product, above crude product was chromatographed on silicagel using ethylacetate as developing solvent. The pure product was viscous oil and showed only one spot (Rf 0.60) on TLC (silicagel; ethylacetate, IR (liquid film) 1670 cm-1, UV λmaxMeOH 268 nm.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US03935221 |
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| 出典データセット | uspto-grants-1976_01 |
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| ORD ID | ord-d9071daa7c4c4822929cdf2ca5e2fa4b |
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| 出典メモ | uspto-grants-1976_01 |
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