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Chemical Structure| 83603-04-7 Chemical Structure| 83603-04-7

Structure of 83603-04-7

Chemical Structure| 83603-04-7

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Product Details of [ 83603-04-7 ]

CAS No. :83603-04-7
Formula : C11H18O4S
M.W : 246.32
SMILES Code : O=S(C[C@]1(C2(C)C)C(CC2CC1)=O)(OC)=O
MDL No. :N/A

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Application In Synthesis of [ 83603-04-7 ]

* 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 [ 83603-04-7 ]

[ 83603-04-7 ] Synthesis Path-Downstream   1~1

  • 1
  • [ 136310-64-0 ]
  • [ 83603-04-7 ]
  • [ 1256081-13-6 ]
YieldReaction ConditionsOperation in experiment
80% In dichloromethane; acetonitrile; at 20℃; for 24h;Product distribution / selectivity; Tiotropium salt with 1 R-(-)-10-camphorsulphonic acid (anhydrous) 9-Methyl-3-oxa-9-azatricyclo[3.3.1.02'4]non-7-yl hydroxy(di-2-thienyl) acetate (0.1 mol) was suspended in a methylene chloride/acetonitrile mixture (76 ml: 115 ml; 1 : 1.5 v/v). To the mixture methyl 1 R-(-)-10-camphorsulphonate (0.5 mol) in 73 ml of acetonitrile was added. Reaction was carried out for 24h at room temperature. Then the reaction mixture was concentrated by evaporation until crystals precipitated and the obtained crystals were triturated in methylene chloride, filtered off and dried in vacuum dryer at 3O0C. Yield: 80%, HPLC purity: 99.74%.[alpha]D20 (methanol, c=1 ) -14.89 +/- 0.77 Elemental analysis: 029H37NO8S3 (FW = 623.8) Calculated: C 55.84 %; H 5.98 %; N 2.25%; S 15.42% Found: C 55.75%; H 6.09%; N 2.27%; S 15.25%.1H NMR (500 MHz) DMSO-d6 delta 0.74 (s, 3H), 1.05 (s, 3H), 1.28 (q, 2H), 1.79 (d, 2H), 1.81 -1.93 (m, 3H), 2.25 (dt, 1 H), 2.37 (d, 1 H), 2.68-2.84 (m, 3H), 2.87 (d, 2H), 3.04 (s, 3H), 3.24 (s, 3H), 3.50 (s, 2H), 4.12 (d, 2H), 5.12 (t, 1 H), 7.01 (t, 2H), 7.13 (t, 2H), 7.43 (s, 1 H), 7.53 (t, 2H).13C NMR (500 MHz) DMSO-d6 delta (ppm): 20.29, 20.88, 24.82, 27.12, 28.99, 42.82, 42.96, 47.34, 54.36, 56.26, 58.96, 64.43, 65.17, 77.01 , 126.51 , 126.88, 127.50, 147.34, 170.44, 217.12.
 

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