Acetone → HCID 135735632, compound

Participants

Reaction Steps

To a mixed solution containing 19 g of 2-(N-tert-butylsulfamoyl)-4-[4-(2-methoxyethoxy)-5-sulfophenylazo]-5-methanesulfonamido-1-naphthol prepared as described in Step (a) above, 100 ml of acetone and 20 ml of phosphorous oxychloride, 20 ml of N,N-dimethylacetamide was added dropwise at a temperature of 50° C. or below. After completion of the dropwise addition, the mixture was stirred for 1 hour and was poured gradually into 500 ml of ice water. The crystals thus-precipitated were collected by filtration, washed with 50 ml of acetonitrile and air-dried.

Provenance & Evidence