Triethylamine → HCID 22609770, compound

Temperature

0 °C

N-Acetylethylenediamine (10.2 g, 100 mmol) and triethylamine (15 ml, 10.9 g, 108 mmol) were dissolved in dichloromethane (300 ml) and the solution cooled to 0° C. Methanesulphonyl chloride (8 ml, 11.8 g, 103 mmol) was dissolved in dichloromethane (10 ml) and added dropwise, and stirring was continued at 0° C. for 3 hours. The dichloromethane was removed in vacuo, and the residue was suspended in a mixture of ether and acetone, removing the insoluble material by filtration. The filtrate was concentrated in vacuo to give the title compound as a pale brown gum (14.5 g, 88.3 mmol, 88%); δH [2H6]DMSO 7.93 (1H,br t), 7.05 (1H,t), 3.11 (2H,t), 2.97 (2H,t), 2.89 (3H,s), 2.09 (3H,s).

1. additionadded dropwise
2. customThe dichloromethane was removed in vacuo
3. additionthe residue was suspended in a mixture of ether and acetone
4. customremoving the insoluble material
5. filtrationby filtration
6. concentrationThe filtrate was concentrated in vacuo

ORD record

ord-0bba58fd23b246f4b8e6968bdba4af67

Source dataset

uspto-grants-2001_03

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US06207669B1