Hydrochloric Acid → N-Nitrosobis(2-methoxyethyl)amine

To the mixture of 133 g of bis(2-methoxyethyl)amine, 145 ml of concentrated HCl (36%) and 400 g of ice, 70 g of sodium nitrite dissolved in 250 ml of water was added dropwise slowly while keeping the reaction temperature at 10° C. or below, and then stirred for 2 hours at 10° C. or less and for further 2 hours at room temperature. 250 g of sodium chloride was added thereto, and the mixture was thrice extracted with 500 ml of ethyl acetate and dried with magnesium sulfate. After removing the solvent, the mixture was purified by a silica gel column by using the mixed solvent (hexane/ethyl acetate: 3/1) to obtain 85 g of bis(2-methoxyethyl)nitrosoamine.

1. additionwas added dropwise slowly
2. customat 10° C. or below
3. extractionextracted with 500 ml of ethyl acetate
4. dry with materialdried with magnesium sulfate
5. customAfter removing the solvent
6. customthe mixture was purified by a silica gel column

ORD-Eintrag

ord-f7915b24e10e46b882da37b3ff282f6f

Quelldatensatz

uspto-grants-1989_01

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US04801521