Phosphoric Acid → HCID 66905503, compound

Participants

Reaction Steps

While a solution obtained by mixing 85% phosphoric acid (143.6 g, 1.2 mol) and acetonitrile (500.0 g) was cooled to not more than 15 degree centigrade and stirred under nitrogen atmosphere, a toluene solution (847.3 g, 3-aminothiophene: concentration; 13.1 weight %, content; 111.0 g, 1.1 mol) of 3-aminothiophene prepared in the same manner as in Example 1 was added dropwise thereto. The precipitated crystal was filtered and washed with acetonitrile (200.0 g). The obtained crystal was suspended in acetonitrile (800.0 g) and stirred in an ice water bath for 1 hour. The crystal was filtered again and washed with acetonitrile (200.0 g). The resulting crystal was dried under reduced pressure to give 148.5 g of 3-aminothiophene phosphate (yield: 68%).

Provenance & Evidence