701209-98-5 synthesis

Yield:701209-98-5 75%

Reaction Conditions:

with toluene-4-sulfonic acid in toluene at 120; for 24 h;

Steps:

1.4 Step 4:

Step 4:
3,4-dimethoxythiophene (5 g, 34 mmol), dibromoneopentyl glycol (18 g, 68 mmol), p-toluenesulfonic acid (0.87 g, 5.1 mmol) and 400 ml of toluene are charged into a flask overhead linked to Soxhlet extractor and react at 120° C. for 24 hrs.
The reaction is cooled to room temperature, washed with water several times, dried over anhydrous sodium sulfate, and rotary-vaporized to remove solvents.
The crude is passed through a separation column, to give a oily liquid, which upon condensation becomes a crystalline material, 3,4-(2,2-dibromomethyl)propylenedioxythiophene (compound 4), yield 75%, purity 95%.

References:

US2016/264595,2016,A1 Location in patent:Paragraph 0058; 0062