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CAS No. : | 23082-50-0 | MDL No. : | MFCD00052836 |
Formula : | C8H6ClNO3 | Boiling Point : | No data available |
Linear Structure Formula : | - | InChI Key : | PNXVQYABDFYOFY-UHFFFAOYSA-N |
M.W : | 199.59 | Pubchem ID : | 89996 |
Synonyms : |
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Signal Word: | Warning | Class: | |
Precautionary Statements: | P261-P305+P351+P338 | UN#: | |
Hazard Statements: | H302-H315-H319-H335 | Packing Group: | |
GHS Pictogram: |
* 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.
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
With hydrogen sulfide; ammonia; | EXAMPLE 6 Preparation of 3-Methyl-5-nitro-1,2-benzisothiazole Ammonia (45 g, 2,642 mmol) is bubbled into methanol at -40 C. in a steel bomb. Sulfur (30.5 g, 95.0 mmol) and 2'-chloro-5'-nitroacetophenone (19 g, 95.0 mmol) are then added. The bomb is sealed and heated at about 90 C. overnight. After cooling, the reaction mixture is removed from the bomb and concentrated in vacuo to obtain a residue. The residue is diluted with methylene chloride, passed through a plug of silica gel and concentrated in vacuo to give the title product as an orange solid (12.0 g) which is identified by NMR spectral analyses. | |
With hydrogen sulfide; ammonia; | EXAMPLE 9 Preparation of 3-Methyl-5-nitro-1,2-benzisothiazole STR94 Ammonia (45 g, 2,642 mmol) is bubbled into methanol at -40 C. in a steel bomb. Sulfur (30.5 g, 95.0 mmol) and 2'-chloro-5'-nitroacetophenone (19 g, 95.0 mmol) are then added. The bomb is sealed and heated at about 90 C. overnight. After cooling, the reaction mixture is removed from the bomb and concentrated in vacuo to obtain a residue. The residue is diluted with methylene chloride, passed through a plug of silica gel and concentrated in vacuo to give the title product as an orange solid (12.0 g) which is identified by NMR spectral analyses. | |
With hydrogen sulfide; ammonia; In methanol; dichloromethane; | EXAMPLE 25 Preparation of 3-Methyl-5-nitro-1,2-benzisothiazole STR94 Anhydrous ammonia (30 g) is added to methanol in a steel bomb cooled in an ice/water bath. After the addition is complete, 2-chloro-5-nitroacetophenone (12.1 g, 60.7 mmol) and sulfur (2.0 g, 62.4 mmol) are added to the reaction mixture. The bomb is sealed, heated at about 80-85 C. overnight, cooled in an ice/water bath and vented. The reaction mixture is diluted with methanol and concentrated in vacuo to obtain a yellow solid. A solution of the yellow solid in methylene chloride is passed through a dry silica gel pad and concentrated in vacuo to yield a solid which is recrystallized from a methylene chloride/hexanes solution to give the title product as a solid, mp 124-125 C. |
With hydrogen sulfide; ammonia; | EXAMPLE 3 Preparation of 3-Methyl-5-nitro-1,2-benzisothiazole Ammonia (45 g, 2,642 mmol) is bubbled into methanol at -40 C in a steel bomb. Sulfur (30.5 g, 95.0 mmol) and 2'-chloro-5'-nitroacetophenone (19 g, 95.0 mmol) are then added. The bomb is sealed and heated at about 90 C overnight. After cooling, the reaction mixture is removed from the bomb and concentrated in vacuoto obtain a residue. The residue is diluted with methylene chloride, passed through a plug of silica gel and concentrated in vacuoto give the title product as an orange solid (12.0 g) which is identified by NMR spectral analyses. | |
With hydrogen sulfide; ammonia; | EXAMPLE 5 Preparation of 3-Methyl-5-nitro-1,2-benzisothiazole Ammonia (45 g, 2,642 mmol) is bubbled into methanol at -40 C. in a steel bomb. Sulfur (30.5 g, 95.0 mmol) and 2'-chloro-5'-nitroacetophenone (19 g, 95.0 mmol) are then added. The bomb is sealed and heated at about 90 C. overnight. After cooling, the reaction mixture is removed from the bomb and concentrated in vacuo to obtain a residue. The residue is diluted with methylene chloride, passed through a plug of silica gel and concentrated in vacuo to give the title product as an orange solid (12.0 g) which is identified by NMR spectral analyses. | |
With octasulfur; ammonia; In methanol; at -40 - 90℃;Sealed bomb; | REFERENCE EXAMPLE 7 Preparation of 3-Methyl-5-nitro-1,2-benzisothiazole ammonia (45 g, 2,642 mmol) is bubbled into methanol at -40 C in a steel bomb.. sulfur (30.5 g, 95.0 mmol) and 2'-chloro-5'-nitroacetophenone (19 g, 95.0 mmol) are then added.. The bomb is sealed and heated at about 90 C overnight.. After cooling, the reaction mixture is removed from the bomb and concentrated in vacuo to obtain a residue.. The residue is diluted with methylene chloride, passed through a plug of silica gel and concentrated in vacuo to give the title product as an orange solid (12.0 g) which is identified by NMR spectral analyses. Using essentially the same procedure, the following compounds are obtained: | |
With hydrogen sulfide; ammonia; | EXAMPLE 35 Preparation of 3-Methyl-5-nitro-1,2-benzisothiazole Ammonia (45 g, 2,642 mmol) is bubbled into methanol at -40 C. in a steel bomb. Sulfur (30.5 g, 95.0 mmol) and 2'-chloro-5'-nitroacetophenone (19 g, 95.0 mmol) are then added. The bomb is sealed and heated at about 90 C. overnight. After cooling, the reaction mixture is removed from the bomb and concentrated in vacuo to obtain a residue. The residue is diluted with methylene chloride, passed through a plug of silica gel and concentrated in vacuo to give the title product as an orange solid (12.0 g) which is identified by NMR spectral analyses. |
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