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[ CAS No. 7117-31-9 ] {[proInfo.proName]}

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Chemical Structure| 7117-31-9
Chemical Structure| 7117-31-9
Structure of 7117-31-9 * Storage: {[proInfo.prStorage]}
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Product Details of [ 7117-31-9 ]

CAS No. :7117-31-9 MDL No. :MFCD00067994
Formula : C9H9NO3S Boiling Point : -
Linear Structure Formula :- InChI Key :-
M.W :211.24 Pubchem ID :-
Synonyms :

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Application In Synthesis of [ 7117-31-9 ]

* 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 [ 7117-31-9 ]

[ 7117-31-9 ] Synthesis Path-Downstream   1~6

  • 1
  • [ 103-71-9 ]
  • [ 7117-31-9 ]
  • [ 36881-68-2 ]
YieldReaction ConditionsOperation in experiment
With triethylamine In dimethyl sulfoxide for 2h; Ambient temperature;
  • 2
  • [ 622-58-2 ]
  • [ 7117-31-9 ]
  • [ 36881-73-9 ]
YieldReaction ConditionsOperation in experiment
With triethylamine In dimethyl sulfoxide for 2h; Ambient temperature;
  • 3
  • [ 2909-38-8 ]
  • [ 7117-31-9 ]
  • [ 36881-71-7 ]
YieldReaction ConditionsOperation in experiment
With triethylamine In dimethyl sulfoxide for 2h; Ambient temperature;
  • 4
  • [ 866010-09-5 ]
  • [ 7117-31-9 ]
YieldReaction ConditionsOperation in experiment
67% With sodium hydride In N,N-dimethyl-formamide at 20℃; for 4h;
0.4 g With sodium hydride In N,N-dimethyl-formamide at 20℃; for 2h; 1.3 Step 3: 1-methyl-2,2-dioxo-2,3-dihydro-1H-2λ6-benzo[c][1,2]thiazin-4-one (Formula 9) 2- (methanesulfonyl-methyl-amino) -benzoic acid ethyl ester and 0.83gWas dissolved in 5mL di-methyl formamide, was added to sodium hydride 0.26g (60%) was stirred at room temperature for 2 hours. After 10mL of water was added to complete the reaction, the reaction mixture is de-extracted three times with ethyl ether. After drying the diethyl ether layer under reduced pressure was purified by silica gel column chromatography (ethyl acetate: hexane = 10: 1) separation and purification, to give 0.4g of the product as a white solid.
  • 5
  • [ 40913-92-6 ]
  • [ 7117-31-9 ]
  • C17H15NO6S2 [ No CAS ]
YieldReaction ConditionsOperation in experiment
Stage #1: 1-methyl-2,2-dioxo-2,3-dihydro-1H-2λ6-benzo[c][1,2]thiazin-4-one With sodium hydride In N,N-dimethyl-formamide at 0℃; for 0.166667h; Inert atmosphere; Stage #2: 4-methylsulfonylbenzoyl chloride In N,N-dimethyl-formamide at 25℃; for 1.33333h; Inert atmosphere; 5.12. General procedure for compounds (15a-15j) General procedure: A solution of compound 13 (1.1 g, 5 mmol) in DMF (10 mL) was added to sodium hydride (0.3 g, 7.5 mmol of a 60% suspension in mineral oil which had been washed with benzene by decantation) at 0 °C. After stirring for 10 min, benzoyl chloride (1.4 g, 10 mmol) was added during 20 min. The solution was stirred at 25 °C for 1 h and then evaporated. The residue was suspended in water and extracted with ethyl acetate. The combined organic phase was dried with anhydrous sodium sulfate, filtered and removed by rotary evaporation to yield 14a as brown viscous oil, which was used in the next step without further purification. A solution of compound 14a (0.9 g, 2.8 mmol) in dichloromethane (10 mL) was added to triethylamine (0.4 g, 4 mmol), 18-crown-6 (71 mg, 0.3 mmol) and potassium cyanide (91 mg, 1.4 mmol). The mixture was stirred at 25 °C for 48 h. The mixture was poured into water and extracted with dichloromethane. The combined organic phase was dried with anhydrous sodium sulfate, filtered and removed by rotary evaporation. The residue was scratched from ethyl acetate and ethanol (1/1 by volume) to give desired product 15a as yellow solid (572 mg, yield: 36%). The rest of compounds were prepared by the similar procedure to 15a. Data for (15a): Yield 36%; light yellow solid; mp 208-210 °C; 1H NMR (400 MHz, CDCl3) δ: 8.19 (dd, J = 8.0, 1.4 Hz, 1H), 7.86 (dd, J = 5.2, 3.3 Hz, 2H), 7.73-7.67 (m, 1H), 7.65-7.59 (m, 1H), 7.53 (dd, J = 10.4, 4.7 Hz, 2H), 7.38-7.31 (m, 1H), 7.23 (d, J = 8.3 Hz, 1H), 3.39 (s, 3H); 13C NMR (100 MHz, CDCl3) δ: 193.2, 177.4, 142.1, 137.2, 135.6, 132.5, 128.2, 128.1, 128.1, 123.9, 120.3, 117.9, 115.2, 32.1; HRMS: calcd for C16H13NO4S [M+H]+ 316.0565, found 316.0640.
  • 6
  • [ 21900-54-9 ]
  • [ 7117-31-9 ]
  • C16H11ClFNO4S [ No CAS ]
YieldReaction ConditionsOperation in experiment
Stage #1: 1-methyl-2,2-dioxo-2,3-dihydro-1H-2λ6-benzo[c][1,2]thiazin-4-one With sodium hydride In N,N-dimethyl-formamide at 0℃; for 0.166667h; Inert atmosphere; Stage #2: 2-chloro-4-fluorobenzoyl chloride In N,N-dimethyl-formamide at 25℃; for 1.33333h; Inert atmosphere; 5.12. General procedure for compounds (15a-15j) General procedure: A solution of compound 13 (1.1 g, 5 mmol) in DMF (10 mL) was added to sodium hydride (0.3 g, 7.5 mmol of a 60% suspension in mineral oil which had been washed with benzene by decantation) at 0 °C. After stirring for 10 min, benzoyl chloride (1.4 g, 10 mmol) was added during 20 min. The solution was stirred at 25 °C for 1 h and then evaporated. The residue was suspended in water and extracted with ethyl acetate. The combined organic phase was dried with anhydrous sodium sulfate, filtered and removed by rotary evaporation to yield 14a as brown viscous oil, which was used in the next step without further purification. A solution of compound 14a (0.9 g, 2.8 mmol) in dichloromethane (10 mL) was added to triethylamine (0.4 g, 4 mmol), 18-crown-6 (71 mg, 0.3 mmol) and potassium cyanide (91 mg, 1.4 mmol). The mixture was stirred at 25 °C for 48 h. The mixture was poured into water and extracted with dichloromethane. The combined organic phase was dried with anhydrous sodium sulfate, filtered and removed by rotary evaporation. The residue was scratched from ethyl acetate and ethanol (1/1 by volume) to give desired product 15a as yellow solid (572 mg, yield: 36%). The rest of compounds were prepared by the similar procedure to 15a. Data for (15a): Yield 36%; light yellow solid; mp 208-210 °C; 1H NMR (400 MHz, CDCl3) δ: 8.19 (dd, J = 8.0, 1.4 Hz, 1H), 7.86 (dd, J = 5.2, 3.3 Hz, 2H), 7.73-7.67 (m, 1H), 7.65-7.59 (m, 1H), 7.53 (dd, J = 10.4, 4.7 Hz, 2H), 7.38-7.31 (m, 1H), 7.23 (d, J = 8.3 Hz, 1H), 3.39 (s, 3H); 13C NMR (100 MHz, CDCl3) δ: 193.2, 177.4, 142.1, 137.2, 135.6, 132.5, 128.2, 128.1, 128.1, 123.9, 120.3, 117.9, 115.2, 32.1; HRMS: calcd for C16H13NO4S [M+H]+ 316.0565, found 316.0640.
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