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1,2-DIMETHOXY-D6-BENZENE synthesis

2synthesis methods
-

Yield:24658-24-0 92%

Reaction Conditions:

with potassium hydroxide in dimethyl sulfoxide at 20;

Steps:

1.1 Step 1.1,2-bis(methoxy-d3)benzene (21b).

To a solution of 1,2-dihydroxybenzene (20a) (30 g, 272.5 mmol) in anhydrous DMSO (250 mL) at room temperature was added KOH (61.2 g, 1090 mmol) followed by methyl iodide-d3 (42.4 mL, 681.1 mmol, Sigma Aldrich, > 99.5% atom D). The reaction mixture was stirred at room temperature overnight. The reaction mixture was diluted with water (800 mL) and extracted with CH2Cl2 (4 x 600 mL). The combined organic layers were washed with water (3 x 1L), dried (Na2SO4), filtered and concentrated under reduced pressure. The residue was dried (vacuum oven) to give 21b (36.4 g, 92%) as a yellow oil.

References:

WO2020/132461,2020,A1 Location in patent:Paragraph 167