ChemicalBook CAS DataBase List 6-AMIDINO-2-NAPHTHOL METHANESULFONATE

6-AMIDINO-2-NAPHTHOL METHANESULFONATE synthesis

4synthesis methods

Product Name:6-AMIDINO-2-NAPHTHOL METHANESULFONATE
CAS Number:82957-06-0
Molecular formula:C12H14N2O4S
Molecular Weight:282.32

52927-22-7 Synthesis

52927-22-7
266 suppliers
$6.00/1g

75-36-5 Synthesis

75-36-5
559 suppliers
$17.92/100G

82957-06-0
206 suppliers
$75.00/100mg

Yield:82957-06-0 53%

Reaction Conditions:

Stage #1:6-cyano-2-naphthol;acetyl chloride in ethanol;tert-butyl methyl ether at 0 - 50; for 10 h;Pinner Imino Ether Synthesis;
Stage #2: with methanesulfonic acid in methanol;tert-butyl methyl etherSolvent;

Steps:

3 Example 3:
Take 800 ml of absolute ethanol in three bottles,The mixture was cooled to 0-5 ° C with stirring and 430 ml of acetyl chloride was added dropwise.Dropping completed, at 0 ~ 5 for a period of time, put 6-cyano-2-naphthol 85 g, 10 ° C for 10 hours, methyl tert-butyl ether was added and stirred for 1 hour to filter,The filter cake was washed with methyl tert-butyl ether, dried and mixed directly with ethanol, heated to 50 ,Dry ammonia was bubbled for 3 hours and evaporated to dryness under reduced pressure to give a yellow solid.The mixture was stirred with saturated sodium bicarbonate solution for a period of time, filtered, washed with water until neutral.Wet products suspended in methanol, dropping a certain amount of methanesulfonic acid solution,Methyl tert-butyl ether was added to precipitate a solid, which was filtered, washed with methyl tert-butyl ether,Recrystallization from ethanol gave 75 g of a yellow solid,The temperature of 227 ° C ~ 230 ° C,Yield 53%.

References:

Beijing Lanbeiwang Bio-pharmaceutical Technology Co., Ltd.;Wan Liuyi;Fu Jifeng;Li Shuming CN103896809, 2017, B Location in patent:Paragraph 0010; 0011; 0012; 0013

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52927-22-7 Synthesis

52927-22-7
266 suppliers
$6.00/1g

82957-06-0
206 suppliers
$75.00/100mg

References

765871-54-3 Synthesis