6-AMIDINO-2-NAPHTHOL METHANESULFONATE synthesis
- Product Name:6-AMIDINO-2-NAPHTHOL METHANESULFONATE
- CAS Number:82957-06-0
- Molecular formula:C12H14N2O4S
- Molecular Weight:282.32
52927-22-7
293 suppliers
$6.00/1g
75-36-5
579 suppliers
$17.92/100G
82957-06-0
218 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
52927-22-7
293 suppliers
$6.00/1g
82957-06-0
218 suppliers
$75.00/100mg
765871-54-3
17 suppliers
inquiry
82957-06-0
218 suppliers
$75.00/100mg
75-75-2
636 suppliers
$10.00/5g
58200-88-7
15 suppliers
inquiry
82957-06-0
218 suppliers
$75.00/100mg