Add tBuOH (38 mL, 0.4 mol) to an ice-cold solution of con. H2SO4 (22 mL, 0.4 mol) in H2O (25.0 mL),dropwise.
Add a solution of sodium nitrite (42.0 g in 100 mL of H2O) to the above solution.
Keep the reaction mixture at approximately 0 °C during the addition.
Warm the reaction mixture to room temperature.
Stir the reaction mixture overnight.
Separate the aqueous layer.
Wash the organic portion with saturated aq. NaHCO3 solution and saturated aq. NaCl solution successively.
Dry the organic layer with anhydrous Na2SO4.
Purify the mixture by distillation.
Collect the tert-butyl nitrite at about 80 °C (ca. 25 mL).
С другой стороны, нашел вот такую инфу - In Bretherick's Handbook of Reactive Chemical Hazards (Seventh Edition), 2007:
Many alkyl nitrites are thermally unstable and may readily decompose or explode on heating [1]. Methyl nitrite explodes more violently than ethyl nitrite [2]. Lower alkyl nitrites have been known to decompose and burst the container, even in refrigerated storage.
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