Ethylenediamine → HCID 14009874, compound

Temperature

20 °C

Ethylenediamine (30 g) was dissolved in 120 g of acetonitrile, and a solution of 17.6 g of 5-bromomethyl-3-methylisoxazole in 30 ml of acetonitrile was added dropwise at 5° to 10° C. After the addition, the mixture was stirred for 1 hour with a care taken not to permit the temperature of the reaction system to rise above 20° C. Then, most of the volatile materials were removed under vacuum (less than 2 mmHg) while maintaining the bath temperature at 20° C. Ice water was added to the residue, and the mixture was extracted with dichloromethane. The dichloromethane layer was dehydrated, and dichloromethane was distilled off under reduced pressure to give 10.0 g of N-(3-methyl-5-isoxazolylmethyl)ethylenediamine (purity about 95%) as a colorless oil.

1. additionAfter the addition
2. customto rise above 20° C
3. customThen, most of the volatile materials were removed under vacuum (less than 2 mmHg)
4. additionIce water was added to the residue
5. extractionthe mixture was extracted with dichloromethane
6. distillationdichloromethane was distilled off under reduced pressure

ORD record

ord-c726ac5c93754950a28075f3db133338

Source dataset

uspto-grants-1998_05

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US05750704