Phosphorus oxychloride → HCID 20531786, compound

Participants

Reaction Conditions

Reaction Steps

10 ml of N,N-dimethylacetoamide was added dropwise to a mixture of 13 g of N,N-diethyl-4-[4-(2-methoxyethoxy)-3-sulfophenylazo]-aniline prepared in Step (1) described above, 100 ml of acetonitrile and 13 ml of phosphorus oxychloride while the reaction mixture was maintained at a temperature of 30° C. or lower. After completion of the addition, the mixture was allowed to stand with stirring over a period of 3 hours and then, it was poured little by little into 500 ml of ice water. The crystals thus precipitated were recovered by filtration, washed with 200 ml of water and air-dried. Yield 11.0 g, Melting Point 103°-104° C.

Provenance & Evidence