반응 #53591

반응 방정식

7-amino-1-hydroxy-3-naphthalene sulfonic acid

sodium hydrosulfite

HCl

sodium sulfanilate

sodium nitrite

→

title compound

수율 45.0%

7,8-Diamino-1-hydroxy-3-naphthalene sulfonic acid dihydrochloride

수율 45.0%

용매

water

water

반응 조건

후처리

1. 1
   온도The reaction mixture was warmed to 50° C.
2. 2
   workup.STIRRINGthe reaction was stirred for 4 hours
3. 3
   여과The reaction was filtered
4. 4
   세척the precipitate was washed with water, methanol, and ether

실험 절차

A stirred solution of p-benzenediazonium sulfonic acid, was prepared by the addition of sodium sulfanilate (1.10 g, 5.2 mmole) to sodium nitrite (0.40 g, 5.7 mmole) in water (10 mL) followed by addition to ice (6.0 g) and concentrated HCl (1.1 mL, 37%). After 30 min. of standing at 0° C. 7-amino-1-hydroxy-3-naphthalene sulfonic acid (1.2 g, 5.2 mmole) was added in water (10 mL) and the reaction was stirred at room temperature overnight. The reaction mixture was warmed to 50° C. and sodium hydrosulfite (3.0 g, 15.6 mmole) was added and the reaction was stirred for 4 hours. The reaction was filtered and the precipitate was washed with water, methanol, and ether to give the title compound (0.54 g; 45%) as a red solid. MS(ES) m/z 255 [M+H].

출처