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HRID 1580975作成日:2026年10月25日

Methylamine → HCID 13298527、化合物

https://huagongshe.com/reaction/1580975

反応式

関与物質

役割名称HCID仕込み量
反応物MethylamineHCID 6329—
反応物Thionyl ChlorideHCID 24386—
反応物5-(3,4-Dibromobutyl)pyridine-2-carboxylic acidHCID 216720—
溶媒ChloroformHCID 6212—
生成物HCID 13298527HCID 13298527—

反応条件

温度8 °C

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

DOI10.6084/m9.figshare.5104873.v1
特許番号US03935221
出典データセットuspto-grants-1976_01
ORD IDord-d9071daa7c4c4822929cdf2ca5e2fa4b
出典メモuspto-grants-1976_01