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Chemical Structure| 15446-25-0 Chemical Structure| 15446-25-0

Structure of 15446-25-0

Chemical Structure| 15446-25-0

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Product Details of [ 15446-25-0 ]

CAS No. :15446-25-0
Formula : C9H9ClO4S
M.W : 248.68
SMILES Code : O=C(OC)CS(=O)(C1=CC=C(Cl)C=C1)=O
MDL No. :MFCD01122030

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Application In Synthesis of [ 15446-25-0 ]

* 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 [ 15446-25-0 ]

[ 15446-25-0 ] Synthesis Path-Downstream   1~2

  • 1
  • [ 14752-66-0 ]
  • [ 96-34-4 ]
  • [ 15446-25-0 ]
YieldReaction ConditionsOperation in experiment
98% In N,N-dimethyl-formamide; at 45 - 115℃; for 3h; A solution of 108.53 g (1 mol) of methyl ester ofmonochloroacetic acid (4) in 200 mL of DMF was addedto a suspension of 198.6 g (1 mol) of <strong>[14752-66-0]sodium 4-chlorophenylsulfinate</strong> (prepared by reacting 4-chlorophenylsulfochloridewith sodium sulfi te in 500 mL of DMF)heated to 45C. The reaction mixture was heated withstirring to 115C for 3 h. After cooling, it was pouredinto 3 L of cold water and held in a refrigerator for 12 h.The precipitate was fi ltered off, recrystallized from chloroform-hexane, and dried over P2O5. 233.7 g (98%) ofester 5 was obtained, mp 81-82C. 1 NMR spectrum, δ, ppm (D3OD): 7.40-7.31 m (4, 64), 4.05 s (2,2), 3.29 s (3, 3). IR spectrum, ν, cm-1:1735 (), 1150, 1330 (SO2). Found, %: C 43.80,H 3.45, Cl 14.11, S 13.12. C9H9ClO4S. Calculated, %:C 43.46, H 3.66, Cl 14.25, S 12.89.
  • 2
  • [ 14752-66-0 ]
  • [ 96-32-2 ]
  • [ 15446-25-0 ]
YieldReaction ConditionsOperation in experiment
77.7% In N,N-dimethyl-formamide; at 80℃; for 2h; Example 5; 7-Chloro-3-(4-chloro-benzenesulfonyl)-4-(4-methyl-piperidin-l-yl)-quinoline; Table I compound 195; (4-Chloro-benzenesulfonyl)-acetic acid methyl ester; The mixture of methyl bromoacetate (11.25 ml, 116 mmol) sodium 4-chloro- benzenesulfinate (25.2g, 116 mmol) in DMF (120 ml) was stirred and heated at 8O0C for 2 h. The solution was diluted with water (360 ml). The separated oil was extracted with chloroform (200 ml) and washed with water (3 X 80 ml). The organic phase was evaporated in vacuo. The yield was 22.4 g (77.7%). MS (EI) M+ = 249.
77.7% In N,N-dimethyl-formamide; at 80℃; for 2h; A mixture of methyl bromoacetate (11.25 ml, 116 mmol) and sodium 4-chloro- benzenesulfinate (25.2g, 116 mmol) in DMF (120 ml) was stirred and heated at 8O0C for 2 h. The solution was diluted with water (360 ml). The separated oil was extracted with chloroform (200 ml) and washed with water (3 X 80 ml). The organic phase was evaporated in vacuo to obtain 22.4 g of the title compound in 77.7% yield. MS (EI) M+ = 249.1.
 

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