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Chemical Structure| 30273-23-5 Chemical Structure| 30273-23-5

Structure of 30273-23-5

Chemical Structure| 30273-23-5

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Product Details of [ 30273-23-5 ]

CAS No. :30273-23-5
Formula : C7H9Cl2N
M.W : 178.06
SMILES Code : NC1=CC=C(Cl)C(C)=C1.[H]Cl
MDL No. :MFCD00143296
InChI Key :OURXVKDUZPXMQX-UHFFFAOYSA-N
Pubchem ID :181991

Safety of [ 30273-23-5 ]

GHS Pictogram:
Signal Word:Warning
Hazard Statements:H302-H315-H319-H335
Precautionary Statements:P261-P264-P270-P271-P280-P301+P312-P302+P352-P304+P340-P305+P351+P338-P330-P332+P313-P337+P313-P362-P403+P233-P405-P501

Application In Synthesis of [ 30273-23-5 ]

* 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 [ 30273-23-5 ]

[ 30273-23-5 ] Synthesis Path-Downstream   1~1

  • 1
  • [ 30273-23-5 ]
  • [ 6291-02-7 ]
YieldReaction ConditionsOperation in experiment
Example 67: 4-Chloro-3-methylsulfonylchloride; [00464] Iron powder (150 g, 2.68 mol) and AcOH (600 mL) were charged into a 2 L round bottom flask equipped with a mechanical stirrer and thermometer. The mixture as warmed to 80 C. 4-Chloro-3-methylnitrobenzene (150 g, 0.87 mol) in AcOH (200 mL) was added slowly to the flask over 4 h, keeping the reaction temperature below 90 C. Upon consumption of the reactants, the mixture was filtered through a pad of Celite and the filter cake was washed with methanol (200 mL). The filtrate was concentrated and the residue was poured into 1.5 L of ice water (1 :1) and the resulting precipitate was filtered. The crude product was dissolved in 300 mL 6N HCI in water/dioxane (1 :1) and stirred at 100 C for 3 h. It was then cooled to room temperature and the precipitate was filtered and dried to provide 130 g of 4-chloro-3-methyl- phenylamine hydrochloride as a colorless powder. [00465] 4-Chloro-3-methylaniline hydrochloride (75 g, 0.54 mol) was dissolved in 200 mL concentrated hydrochloride acid (200 mL) and acetic acid (60 mL). The mixture was cooled to -5 C and NaNO2 (40.9 g, 0.59 mmol) was added. The mixture was stirred between -10 C to -5 C for 1 h. While the EPO <DP n="142"/>diazotization was in progress, glacial AcOH (600 mL) was placed in a 4000-mL beaker and stirred magnetically. Sulfur dioxide was introduced by a bubbler tube with a fritted end immersed below the surface of the AcOH until saturation was evident. Cuprous chloride (15 g) was added to the solution. The introduction of sulfur dioxide was continued until the yellow-green suspension becomes blue- green. The mixture was then placed in an ice bath and cooled to 10 C. The diazotization reaction mixture was subsequently added in portions over a 30 min period to the sulfur dioxide solution, ensuring the temperature of the solution did not exceed 30 C. After all the diazonium salt mixture was added, the mixture was poured into ice water (2 L). The resulting precipitate was filtered and re- dissolved in hexane (500 mL). The mixture was filtered through a pad of silica gel (100 g) and the filter pad was washed with hexane (300 mL). The combined filtrate was concentrated to yield 50 g of 4-chloro-3~methylbenzenesulfonyl chloride as slightly yellow solid.
 

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