ChemicalBook CAS DataBase List Sodium 4-amino-1-naphthalenesulfonate

Sodium 4-amino-1-naphthalenesulfonate synthesis

4synthesis methods

Product Name:Sodium 4-amino-1-naphthalenesulfonate
CAS Number:130-13-2
Molecular formula:C10H10NNaO3S
Molecular Weight:247.24

The preparation of Sodium 4-amino-1-naphthalenesulfonate is as follows:To a suspension of 4-amino-l -naphthalene sulfonic acid (10.Og, 44.8 mmol) in 10 ml MeOH was added 5 N NaOMe (9 ml). The mixture was sonicated to effect complete solution. The solvent was evaporated to provide the sodium salt of -amino-1- naphthalene sulfonic acid as a white solid. This solid was suspended in 100 ml acetic anhydride and heated at 110 °C for 2 1/2 h. Adding some MeOH to the cooled mixture and co-evaporating with 3x100 ml toluene gave the Na-salt of 4-acetamidonaphthalene-l -sulfonic acid as a white powder.

134-32-7
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$9.00/1g

130-13-2
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$7.00/10g

Yield:-

Reaction Conditions:

Stage #1:1-amino-naphthalene with sulfur trioxide in 1,2-dichloro-benzene at 40; for 0.833333 h;Large scale;
Stage #2: with sodium hydroxide in water;1,2-dichloro-benzene; pH=7 at 85 - 190; for 3 h;Autoclave;Large scale;Temperature;Solvent;Reagent/catalyst;

Steps:

2 Example 2:
The gas SO3 is cooled to 45 ° C with a dew point of less than -50 ° C dry air mixed,Forming a mixed gas of SO3 in a volume ratio of 7%The mixture is passed to the raw material1-naphthylamine (3.75 Kg), o-dichlorobenzene (9 L)And bothTetramethylbenzene(5L)Of the reactor,Where n SO3 / n1-naphthylamine = 1.4: 1,The reaction was carried out at 40 ° C for 50 min to form a sulfonated salt,After the sulfonation reaction,Stop the mixture of SO3 and air; then,The reactor was heated to 190 ° C for 180 min,Water (11 L) was slowly added to the autoclave,To a temperature drop to 85 ° C, solid sodium hydroxide (1.13 Kg) was added to neutralize the mixture to a pH of 7,After the solution was separated, the oil phase and the aqueous phase were obtained. The aqueous phase was concentrated until the specific gravity of the concentrate was 1.21,The resulting concentrated solution was allowed to stand at 65 ° C for 1 hour and then separated,To give the product 1-naphthylamine-4-sulfonate.Product quality yield of 1.72,The total amino value of the product was 78.4% according to HG / T 3387-1999.

References:

China Daily-Use Chemistry Industry Academe;Li, Ping;Yang, Xiaoyi;Guo, Chaohua;Li, Quanhong;Li, Jianbo;Lu, Jianqiang;Li, Huifang;Geng, Weidong;Yang, Xiaodong;Cen, Shiming CN106243001, 2016, A Location in patent:Paragraph 0012; 0013; 0014; 0015; 0016; 0017