N-(4-methylphenyl)sulfonyloxypropan-2-imine synthesis

Yield:67342-52-3 93%

Reaction Conditions:

Stage #1: acetonewith hydroxylamine hydrochloride;sodium hydrogencarbonate at 0; for 1.5 h;
Stage #2: p-toluenesulfonyl chloride at 0; for 2 h;Temperature;

Steps:

1-3 Example 2 Synthesis of Acetone oxime-O-p-methanesulfonate

20 g of hydroxylamine hydrochloride (Compound II, 0.29 mol),Acetone 200ml (2.7mol), temperature control 0 ° C, adding 40 g (0.48 mol) of sodium bicarbonate,After stirring for 1.5 h, 15 g (0.078 mol) of p-toluenesulfonyl chloride was added.Continue to control the temperature at 0 ° C, react for 2 h, add 400 ml of water and stir to precipitate a large amount of solids.After suction filtration, the mixture was dried under reduced pressure at 35 ° C to yield 13.7 g (0.06 mol) of white solid.The yield was 91.5%.Add 10 g of crude acetone -O-p-methanesulfonate to a single-mouth bottle.Add 80 ml of 60% acetone aqueous solution, stir at 0 to 10 ° C for 1 h.After suction filtration and drying, 9.3 g of a white solid was obtained, yield 93.0%, purity 99.5%.

References:

CN109134331,2019,A Location in patent:Paragraph 0032-0040