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Chemical Structure| 133777-96-5 Chemical Structure| 133777-96-5

Structure of 133777-96-5

Chemical Structure| 133777-96-5

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Product Details of [ 133777-96-5 ]

CAS No. :133777-96-5
Formula : C18H21NO4S
M.W : 347.43
SMILES Code : N(S(=O)(=O)C=C)(CC1C=CC(=CC=1)OC)CC1C=CC(=CC=1)OC
MDL No. :MFCD31560374

Safety of [ 133777-96-5 ]

GHS Pictogram:
Signal Word:Warning
Hazard Statements:H302-H315-H319
Precautionary Statements:P501-P270-P264-P280-P302+P352-P337+P313-P305+P351+P338-P362+P364-P332+P313-P301+P312+P330

Application In Synthesis of [ 133777-96-5 ]

* 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 [ 133777-96-5 ]

[ 133777-96-5 ] Synthesis Path-Downstream   1~2

  • 1
  • [ 337529-74-5 ]
  • [ 133777-96-5 ]
  • methyl α-[2-[[bis[(4-methoxyphenyl)methyl]amino] sulfonyl]ethyl]-2-fluoro-4-nitrobenzeneacetate [ No CAS ]
YieldReaction ConditionsOperation in experiment
81% With potassium carbonate;18-crown-6 ether; In toluene; for 3h;Heating / reflux; Step 1 Preparation of methyl alpha-[2-[[bis[(4-methoxyphenyl)methyl]amino] sulfonyl]ethyl]-2-fluoro-4-nitrobenzeneacetate Methyl 2-(2-fluoro-4-nitrophenyl)acetate (25.0 g, 117.4 mmol), vinyl sulfonamide (35.0 g, 100.9 mmol), anhydrous potassium carbonate (10.0 g, 72.5 mmol) and 18-crown-6 (2.64 g, 10.0 mmol) are heated under reflux in toluene (250 ml) for 3 hr. After cooling, ethyl acetate (500 ml) and water (300 ml) are added. The organic layer is washed with brine (200 ml), dried over MgSO4, filtered and evaporated. The resultant oil is chromatographed over silica gel (1 kg) eluting with 25-50% ethyl acetate-hexane. The title compound is obtained as white crystals (45.8 g, 81%) mp 79.
  • 2
  • [ 6608-47-5 ]
  • [ 854391-95-0 ]
  • [ 133777-96-5 ]
YieldReaction ConditionsOperation in experiment
With triethylamine; In dichloromethane; at 20℃; for 2h; Scheme 1; Methods B and C; Choroethylsulfonyl chloride (3.4 g, 0.02 mol) was dissolved in dichloromethane (100 ml_) and cooled to -780C under nitrogen. Triethylamine (2.12 g, 1 eq) was added and the reaction was stirred at -780C for 10 minutes. The reaction mixture was warmed to room temperature and stirred for 2 hours. Bis-4-methoxydibenzyl- amine.HCI (6 g, 0.02 mol) was added, followed by triethylamine (4.24 g, 2 eq) and the mixture was stirred at room temperature for 2 hours. The reaction mixture was diluted with dichloromethane (100 ml_) and washed with 10% HCI and brine. The solvent was removed in vacuo and the product was isolated by silica gel chromatography using a gradient of 0-50% ethyl acetate/hexane mixture as eluent to afford 1.37 g of compound 2. 1H-NMR (CDCI3 400 MHz) delta 7.25 (d, 4H), 6.87 (d, 4H), 6.26 (m, 2H), 5.86 (d, 1 H), 4.19 (s, 4H)1 3.81 (s, 6H).
 

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