Ethylenediamine → N1-(pyridin-4-yl)ethane-1,2-diamine

The starting material can be prepared as follows: A mixture of 38.9 g of 4-bromo-pyridine-hydrochloride and 480 g of ethylenediamine is refluxed with stirring for 13 hours. The reaction mixture is thereafter concentrated under reduced pressure and the residue is treated with toluene and concentrated once more. The residue is made alkaline with a concentrated aqueous solution of sodium hydroxide and extracted with five 75 ml portions of methylene chloride. The combined extracts are dried over sodium sulphate and concentrated under reduced pressure. Recrystallisation of the residue from methylene chloride yields 4-(2-aminoethylamino)-pyridine as a light yellow crystalline substance with a melting point of 120°-121° C.

1. customThe starting material can be prepared
2. temperatureis refluxed
3. concentrationThe reaction mixture is thereafter concentrated under reduced pressure
4. additionthe residue is treated with toluene
5. concentrationconcentrated once more
6. extractionextracted with five 75 ml portions of methylene chloride
7. dry with materialThe combined extracts are dried over sodium sulphate
8. concentrationconcentrated under reduced pressure
9. customRecrystallisation of the residue from methylene chloride

ORD 기록

ord-fc6a9eb32d5f43d18f9680b39e3d85c1

출처 데이터셋

uspto-grants-1980_08

DOI

10.6084/m9.figshare.5104873.v1

특허 번호

US04217350