3,3-dimethylthiomorpholine

Conditions: temp:0.00; pressure:0.00; stir:

Conditions: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

Procedure: 12 ml of 10N HCl are added with cooling to a mixture of 15.7 g of 3,3-dimethyltetrahydro-1,4-thiazine (step c) and 60 ml of ice-water. A solution of 12.4 g of sodium nitrite in 40 ml of water is then added dropwise at 4° to 6° C. The mixture is subsequently stirred at room temperature for 4 hours, rendered alkaline with potassium carbonate and extracted by shaking with ethyl acetate. The organic phase is dried and concentrated in a water jet vacuum. Yield: 17.5 g; M.p.: yellow oil. extracted by shaking with ethyl acetate The organic phase is dried concentrated in a water jet vacuum

Conditions: temp:0.00; pressure:0.00; stir:

Conditions: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

Procedure: 12 ml of 10N HCl are added with cooling to a mixture of 15.7 g of 3,3-dimethyltetrahydro-1,4-thiazine (step c) and 60 ml of ice-water. A solution of 12.4 g of sodium nitrite in 40 ml of water is then added dropwise at 4° to 6° C. The mixture is subsequently stirred at room temperature for 4 hours, rendered alkaline with potassium carbonate and extracted by shaking with ethyl acetate. The organic phase is dried and concentrated in a water jet vacuum. Yield: 17.5 g; M.p.: yellow oil. extracted by shaking with ethyl acetate The organic phase is dried concentrated in a water jet vacuum