Methylamine → HCID 13298527, 화합물

HRID 1580975

반응식

HRID 1580975 반응식
[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

참가 물질

5

반응물 3

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

생성물 1

HCID 13298527HCID 13298527, 화합물

시약·촉매·용매 1

HCID 6212Chloroform용매

반응 조건

온도
8 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-d9071daa7c4c4822929cdf2ca5e2fa4b
출처 데이터셋
uspto-grants-1976_01
특허 번호
US03935221

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