Tetramethylurea → [Chloro(dimethylamino)methylidene]-dimethylazanium chloride

49.4 g of tetramethylurea were dissolved in 400 ml of 1,2-dichloroethane and 30.0 g of oxalyl chloride were added dropwise to the solution at room temperature over a period of 15 minutes. The resulting solution was stirred at room temperature for 15 minutes and further stirred in an oil bath at 65° C. for 2 hrs. The reaction mixture was concentrated under reduced pressure to 200 ml and allowed to cool, upon which crystals separated out. The crystals were obtained by filtration, washed with ether and dried under reduced pressure to obtain 30.0 g of a white, hygroscopic intermediate.

1. stirringfurther stirred in an oil bath at 65° C. for 2 hrs
2. concentrationThe reaction mixture was concentrated under reduced pressure to 200 ml
3. temperatureto cool, upon which crystals
4. customseparated out
5. customThe crystals were obtained by filtration
6. washwashed with ether
7. customdried under reduced pressure
8. customto obtain 30.0 g of a white, hygroscopic intermediate

ORDレコード

ord-6b50e7f962544730b4bc7a139fde7aa0

出典データセット

uspto-grants-1997_06

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US05637439