Home Cart Sign in  
Chemical Structure| 203731-39-9 Chemical Structure| 203731-39-9

Structure of 203731-39-9

Chemical Structure| 203731-39-9

*Storage: {[sel_prStorage]}

*Shipping: {[sel_prShipping]}

,{[proInfo.pro_purity]}

4.5 *For Research Use Only !

{[proInfo.pro_purity]}
Cat. No.: {[proInfo.prAm]} Purity: {[proInfo.pro_purity]}

Change View

Size Price VIP Price

US Stock

Global Stock

In Stock
{[ item.pr_size ]} Inquiry {[ getRatePrice(item.pr_usd,item.pr_rate,item.mem_rate,item.pr_is_large_size_no_price, item.vip_usd) ]}

US Stock: ship in 0-1 business day
Global Stock: ship in 5-7 days

  • {[ item.pr_size ]}

In Stock

- +

Please Login or Create an Account to: See VIP prices and availability

US Stock: ship in 0-1 business day
Global Stock: ship in 2 weeks

  • 1-2 Day Shipping
  • High Quality
  • Technical Support
Product Citations

Alternative Products

Product Details of [ 203731-39-9 ]

CAS No. :203731-39-9
Formula : C6H5Cl2NS
M.W : 194.08
SMILES Code : CSC1=CN=C(Cl)C(Cl)=C1

Safety of [ 203731-39-9 ]

Application In Synthesis of [ 203731-39-9 ]

* All experimental methods are cited from the reference, please refer to the original source for details. We do not guarantee the accuracy of the content in the reference.

  • Downstream synthetic route of [ 203731-39-9 ]

[ 203731-39-9 ] Synthesis Path-Downstream   1~2

  • 1
  • [ 624-92-0 ]
  • [ 98121-41-6 ]
  • [ 203731-39-9 ]
YieldReaction ConditionsOperation in experiment
With tert.-butylnitrite; In ice-water; hexane; dichloromethane; Precursor alpha: 2,3-Dichloro-5-methylthiopyridine A solution of 50.6 g (0.3 mol) of <strong>[98121-41-6]3-amino-5,6-dichloropyridine</strong> in 700 ml of methylene chloride was slowly added dropwise at 40 C. to a solution of 56.6 g (0.6 mol) of dimethyl disulfide and 46.7 g (0.45 mol) of tert-butyl nitrite in 320 ml of dry methylene chloride. The mixture was then stirred for 1 hour at 40 C. and subsequently for another approximately 15 hours at approximately 20 C., whereupon 500 ml of ice-water were added to the reaction mixture. The organic phase which was separated off was washed once with 1 N hydrochloric acid and once with water, dried over sodium sulfate and finally concentrated. After the crude product had been stirred with n-hexane, 21 g of a dark solid were obtained (purity 94% according to GC). After the hexane solution was concentrated, a further 21.3 g of product of value remained which had a purity of 77% (according to GC). Total yield: 62%; m.p.: 66-67 C.; 1H-NMR (in d6 dimethyl sulfoxide): delta [ppm]=2.6 (s, CH3); 8.1 and 8.3 (2*d, pyr H).
  • 2
  • [ 98121-41-6 ]
  • [ 5188-07-8 ]
  • [ 203731-39-9 ]
YieldReaction ConditionsOperation in experiment
2.85 Example 85 (Prepared according to Scheme 15); (/?)-4-(3-Chloro-5-(methylsulfonyl)pyridine-2-yl)-2-methyl-N-(4-(trimethylsilyl)phenyl)piperazine-l- carboxamide; To a solution of <strong>[98121-41-6]3-amino-5,6-dichloropyridine</strong> (6.13mmol) in HCl (37%, 5ml) at 00C was added sodium nitrite (9.20mmol) in water (2ml) in a dropwise fashion. The reaction was stirred at 00C for 1 hr. The reaction was filtered to remove sodium chloride. A suspension of sodium methanethiolate (7.36mmol) and copper (II) tetrafluoroborate hydrate (0.061mmol) in acetonitrile (5 ml) was cooled to 00C. The solution of the diazonium salt was added dropwise with much nitrogen evolution. The resulting orange suspension was stirred at room temperature for 4 hours. The reaction was quenched with NaOH (50ml) and extracted with ethyl acetate (2x50ml). The organics were combined, washed with brine, dried (MgSO4) and concentrated under reduced pressure. The resulting residue was purified by flash chromatography (0-30% ethyl acetate in petroleum ether) yielding the product 2,3-dichloro-5-(methylthio)pyridine (3.77mmol) 1H NuMR (400 MHz, CDCl3) delta 8.16 - 8.34 (m, IH), 7.59 - 7.76 (m, IH), 2.59 (s, 3H)A solution of 2,3-dichloro-5-(methylthio)pyridine (3.77mmol) in DCM was cooled to 00C. To this was added mCPBA (7.53mmol) the reaction was warmed to room temperature and stirred for 48hr. The reaction was quenched with sat. sodium bicarbonate (50 ml) and extracted with DCM (50 ml x 2) the organic phases were combined, washed with brine, dried (phase separation cartridge) and concentrated under reduced pressure. The resultant white solid was purified by flash chromatography (0-30 % ethyl acetate in petroleum ether) yielding 2,3-dichloro-5-(methylsulfonyl)pyridine (3.72mmol). 1H NuMR (400 MHz, CDCl3) delta 8.61 - 8.99 (m, IH), 8.09 - 8.47 (m, IH), 3.08 (s, 3H).The title compound was synthesized in accordance with Example 23 from the intermediate described above. MS: ES+ 481.1. 1H NuMR (400 MHz, CDCl3) delta 8.62 - 8.69 (m, IH), 8.03 - 8.10 (m, IH), 7.43 - 7.55 (m, 2H), 7.32 - 7.43 (m, 2H), 6.37 (s, IH), 4.35 - 4.48 (m, IH), 4.17 - 4.29 (m, IH), 4.05 - 4.17 (m, IH), 3.93 - 4.03 (m, IH), 3.43 - 3.57 (m, IH), 3.33 - 3.43 (m, IH), 3.13 - 3.26 (m, IH), 3.1 1 (s, 3H), 1.35 - 1.46 (m, 3H), 0.27 (s, 9H)
 

Historical Records