反应 #3682921
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openreactiondata ↗doi:10.6084/m9.figshare.5104873.v1; patent:US05053072
反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: A Grignard solution of 30.5 g of 2-ethoxybenzyl chloride and 6.1 g of magnesium shavings in 250 ml of diethyl ether is added dropwise at -60° C. to -70° C. to 50 ml of sulfur dioxide. Stirring is continued for 0.5 hour at -70° C., the mixture is allowed to come to room temperature, and the salt magnesium 2-ethoxybenzylsulfinate which has formed (47 g, melting point: 134°-139° C., decomposition) is filtered off with suction. The sulfinate salt is dissolved in 900 ml of water and 16.4 g of anhydrous sodium acetate. To this are added 22.7 g of hydroxylamine-O-sulfonic acid at room temperature with stirring. After the mixture has been stirred for 12 hours, the product is filtered off with suction and dried in vacuo. This gives 23.9 g of 2-ethoxybenzylsulfonamide of melting point: 92°-93° C. to come to room temperature
来源 ID: ord-6781643c2f7540f0b65348b3ee2aa6f8