Triethylamine → HCID 19873524、化合物

5.75 g (58.9 mmol) of N,O-dimethylhydroxylamine hydrochloride was suspended in 300 ml of dichloromethane, and 11.9 g (118 mmol) of triethylamine was added thereto. Then, the mixture was cooled with ice, and a dichloromethane solution of 7.63 g of methylsulfamoyl chloride was dropwise added, and the mixture was stirred at room temperature for 3 hours. The solvent was distilled off under reduced pressure. To the residue, 200 ml of benzene was added, and insoluble substance was filtered off. Then, the solvent was distilled off again under reduced pressure. By the distillation under reduced pressure, 4.4 g of N,N'-dimethyl-N'-methoxysulfamide was obtained (boiling point: 85°-88° C./1.9 mmHg).

1. temperatureThen, the mixture was cooled with ice
2. distillationThe solvent was distilled off under reduced pressure
3. additionTo the residue, 200 ml of benzene was added
4. filtrationinsoluble substance was filtered off
5. distillationThen, the solvent was distilled off again under reduced pressure
6. distillationBy the distillation under reduced pressure

ORDレコード

ord-3e77ea546b56477dac491051c221d652

出典データセット

uspto-grants-1992_10

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US05152824