2-Amino-5-hydroxynaphthalene-1,7-disulphonic acid → Sulfanilic acid

4-Nitro-o-sulfanilic acid is diazotized and coupled neutrally to I acid. 43 mmol of this dye are dissolved in 200 ml water and indirectly diazotized. After stirring for 1 hour, the excess nitrous acid is removed with amidosulfonic acid and a solution of 43 mmol 4-hydroxy- 7-aminonaphthalene-2,8-disulfonic acid in 200 ml water is added. Coupling is completed overnight at pH 8-9, the dye is filtered under suction and the sulfo groups are split off by boiling for 12 h in a 1:1 mixture of water and N-methyl pyrrolidone containing 60 ml concentrated hydrochloric acid. This dye is diazotized and added dropwise to a solution in 100 ml water of 7.2 mmol of a dye obtained by acidic coupling of p-sulfanilic acid onto 4-amino-5-hydroxynaphthalene sulfonic acid. After stirring overnight, the dye is precipitated by addition of acetone, optionally dissolved and allowed to crystallize once more and then washed with aqueous acetone. 0.1 g dye are dissolved in 9.9 g Mowiol® 28-99 (a product of Hoechst AG) and 190 ml water and a 500μ thick layer is cast from this solution. After evaporation of the water, an approx. 50μ thick dark-blue film is obtained. The film is stretched by 500% at 130° C. The dichroic ratio (CR) is 15.3 at 650 nm.

1. customthe excess nitrous acid is removed with amidosulfonic acid
2. waitCoupling is completed overnight at pH 8-9
3. filtrationthe dye is filtered under suction
4. customthe sulfo groups are split off
5. additionby boiling for 12 h in a 1:1 mixture of water and N-methyl pyrrolidone containing 60 ml concentrated hydrochloric acid
6. additionadded dropwise to a solution in 100 ml water of 7.2 mmol of a dye

ORDレコード

ord-80405a6d202c492785d5d8c257f95b45

出典データセット

uspto-grants-1994_08

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US05340504