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[ CAS No. 40248-84-8 ] {[proInfo.proName]}

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Chemical Structure| 40248-84-8
Chemical Structure| 40248-84-8
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Product Details of [ 40248-84-8 ]

CAS No. :40248-84-8 MDL No. :MFCD01317829
Formula : C6H6OS Boiling Point : No data available
Linear Structure Formula :- InChI Key :DOFIAZGYBIBEGI-UHFFFAOYSA-N
M.W : 126.18 Pubchem ID :2736613
Synonyms :

Safety of [ 40248-84-8 ]

Signal Word:Danger Class:9
Precautionary Statements:P280-P305+P351+P338-P273 UN#:3334
Hazard Statements:H317-H318-H410 Packing Group:Ⅲ
GHS Pictogram:

Application In Synthesis of [ 40248-84-8 ]

* 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 [ 40248-84-8 ]

[ 40248-84-8 ] Synthesis Path-Downstream   1~3

  • 1
  • [ 67442-07-3 ]
  • [ 40248-84-8 ]
  • [ 853645-32-6 ]
YieldReaction ConditionsOperation in experiment
With potassium carbonate; In N,N-dimethyl-formamide; at 23℃; Hepta-2,6-dienoic acid methoxy-methyl-amide (2-114): To a solution of 2-chloro-.V-methoxy- //-methylacetamide (6.0 g, 48.8 mmol) in dry DMF (20 mL) at 23 0C was added 3- mercaptophenol (4.44 mL, 48.8 mmol) and K2CO3 (6.7 g, 48.8 mmol). The resulting suspension was stirred at 23 0C overnight. After this period of time, Merrifield resin (24 g, < 2 mmol.g"1, < 48.8 mmol) was added to the mixture followed by K2CO3 (11.4 g, 83.0 mmol) as well as TBAI (catalytic amount), and the suspension was heated up to 50 0C. After 12 hours at this temperature, the resin was filtered and washed several times: HClaq. (50 mL), MeOH (50 mL), CH2Cl2 (50 mL) and Et2O (50 mL). The resin was dried under reduced pressure to constant mass of 29.2 g. The final mass gain (5.2 g, 27.3 mmol) indicated an estimate loading of 0.81 mmol.g"1. Resin 2-49 (10 g, 0.81 mmol.g"1) was suspended in a 1:1 mixture of HFIEVCH2Ch (50 mL). To this suspension, H2O2 (3 mL, 16.0 mmol) was added at 23 0C and the resulting mixture was shaken for 12 h. Resin 2-113 was then filtered, washed using MeOH (50 mL), CH2Cl2 (50 mL) and Et2O (50 mL) and dried under reduced pressure to constant mass before subsequent use. Resin 2-113 (4.0 g, < 0.81 mmol.g"1) was suspended in DMSO (40 mL) followed by the addition of ?BuOK (336 mg, 3.0 mmol). After shaking the reaction for 1 h at room temperature, 5-iodo-l-pentene (588 mg, 3.0 mmol) was added to the suspension and the mixture was shaken for 3 h. The resin was filtered, washed and dried as before. Then, it was suspended in toluene and heated at 80 0C. After 8 h at this temperature, <n="171"/>the resin was filtered and washed several times with more toluene. The combined toluene solutions were evaporated giving pure compound 2-114 as a colourless oil (321 mg, 77 percent) of 95 percent purity judged by NMR. 1H NMR (400 MHz, CDCl3, 25 0C): delta = 6.94 (dt, / = 15.7, 6.7 Hz, IH), 6.39 (d, J = 15.2 Hz, IH), 5.84-5.74 (m, IH), 5.02 (dd, J = 17.4, 1.7 Hz, IH), 4.97 (d, J = 10.1 Hz, IH), 3.67 (s, 3H), 3.21 (s, 3H), 2.34-2.29 (m, 2H), 2.23-2.18 (m, 2H); 13C NMR (100 MHz, CDCl3, 25 0C): 6 = 166.8, 146.7, 137.3, 119.1, 115.3, 61.6, 32.3, 31.7, (one carbon is not detected); LR. (film): Vm3x = 2934, 1681 , 1638, 1378, 1179 cm"1.
  • 2
  • [ 40248-84-8 ]
  • [ 2106-50-5 ]
  • [ 100-39-0 ]
  • [ 1007165-67-4 ]
YieldReaction ConditionsOperation in experiment
37% (3-(Benzyloxy)phenyl)(3~chloro-4-nUrophenyl)sulfane (2a); <n="78"/>The product was purified by silica gel column chromatography using the Combi- Flash system (Hex:EtOAc) as yellowish oil in 37% (1.10 g). Proton NMR and LC analyses confirmed the desired product with purity greater than 95%. TLC (1 :4 EtOAc:Hex), Rf= 0.6; 1H NMR (400 MHz, CDCl3) delta 7.78 (d, IH5 J= 8.4 Hz)3 7.31-7.43 (m, 6H), 7.20 (d, IH, J= 2.0 Hz), 7.05-7.10 (m, 3H), 7.02 (dd, IH, J= 8.4 Hz, J= 1.6 Hz), 5.08 (s, 2H).
  • 3
  • [ 40248-84-8 ]
  • [ 15540-81-5 ]
  • [ 1374025-94-1 ]
YieldReaction ConditionsOperation in experiment
EXAMPLE 4; Preparation of 2-nitro-5- (3-hydroxyphenylthio) -p-xylene [nitroderivative of formula (IV) ]; A mixture of 18.9 g of 3-mercaptophenol (0.150 moles), 32.9 g of <strong>[15540-81-5]2-nitro-5-bromo-p-xylene</strong> (0.143 moles) and K2C03 (0.143 moles) in 95 ml of N,N- dimethylformamide is stirred at room temperature for 2 hours. A solution of HC1 at 10% is added under stirring; the mixture is diluted with ?0 and extracted with ethyl acetate. The organic phase is washed again with water, anhydrified on sodium sulfate, filtered and evaporated. 20 g of solid product are obtained, which is used as such for the subsequent reaction.GC-MS: M+ = 275
20 g With potassium carbonate; In N,N-dimethyl-formamide; at 20℃; for 2h; EXAMPLE 4 Preparation of 2-nitro-5-(3-hydroxyphenylthio)-p-xylene [nitroderivative of formula (IV)] A mixture of 18.9 g of 3-mercaptophenol (0.150 moles), 32.9 g of <strong>[15540-81-5]2-nitro-5-bromo-p-xylene</strong> (0.143 moles) and K2CO3 (0.143 moles) in 95 ml of N,N-dimethylformamide is stirred at room temperature for 2 hours. A solution of HCl at 10% is added under stirring; the mixture is diluted with H2O and extracted with ethyl acetate. The organic phase is washed again with water, anhydrified on sodium sulfate, filtered and evaporated. 20 g of solid product are obtained, which is used as such for the subsequent reaction. GC-MS: M+=275
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