Methylamine → HCID 13298527、化合物

HRID 1580975

反応式

HRID 1580975 の反応式
[CH3:1][NH2:2].[Br:3][CH:4]([CH2:16][Br:17])[CH2:5][CH2:6][C:7]1[CH:8]=[CH:9][C:10]([C:13](O)=[O:14])=[N:11][CH:12]=1.S(Cl)(Cl)=O>C(Cl)(Cl)Cl>[CH3:1][NH:2][C:13](=[O:14])[C:10]1[CH:9]=[CH:8][C:7]([CH2:6][CH2:5][CH:4]([Br:3])[CH2:16][Br:17])=[CH:12][N:11]=1

参加物

5

反応物 3

HCID 6329MethylamineHCID 24386Thionyl ChlorideHCID 2167205-(3,4-Dibromobutyl)pyridine-2-carboxylic acid

生成物 1

HCID 13298527HCID 13298527、化合物

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒

反応条件

温度
8 °C

実験手順

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.

後処理

  1. customChloroform layer which was separated
  2. washwas washed with 0.3% aqueous hydrochloride solution, 5% aqueous sodium bicarbonate solution
  3. customChloroform was evaporated in reduced pressure

出典と根拠

ORDレコード
ord-d9071daa7c4c4822929cdf2ca5e2fa4b
出典データセット
uspto-grants-1976_01
特許番号
US03935221

関連ノート

読み込み中…