PURPOSE: To safely and readily recover the subject compound as an intermediate for N,O-Dimethylhydroxyamine without using an organic solvent by subjecting an N,O-dimethylhydroxycarbamic acid ester and water to azeotropic distillation.
CONSTITUTION: An N,O-dimethylhydorxycarbamic acid ester of the formula (R1 is lower alkyl) and water are subjected to azeotropic distillation preferably under 10-250mmHg at 30-80°C. The amount of water required for azeotropy is an amount to give the ratio of water to the compound of the formula of 1-1.1 to 1 by weight. The compound of the formula, for example, is obtained by reacting hydroxylamine sulfate with a dialkyl carbonate in the presence of NaOH and reacting the reaction product with a methylating reagent such as dimethyl sulfate.
TAKEI MITSUSACHI
KIHARA NORIAKI