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2,2-DIMETHYL-5-NITRO-1,3-DIOXANE synthesis

4synthesis methods
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Yield:4064-87-3 92%

Reaction Conditions:

Stage #1: 2,2-dimethyl-5-hydroxymethyl-5-nitro-1,3-dioxanewith sodium hydroxide in water at 60; for 1 h;
Stage #2: with acetic acid in water at 5; pH=5;

Steps:

2

5-Nitw-2,2-dimethyl-l,3-dioxane is made by mixing 5-nitro-2,2-dimethyl-5- hydroxymethyl-l,3-dioxane (0.03 moles) with about 70 mL of 10 wt. % sodium hydroxide solution, and the solution is stirred at 60°C for about 60 minutes. The solution is cooled to about 5°C, and is acidified to pH 5 with concentrated acetic acid. The precipitated solid is filtered off and dried to give a 92% yield of product.

References:

WO2012/138494,2012,A1 Location in patent:Page/Page column 8