6-Benzoxazolesulfonylchloride,2,3-dihydro-3-methyl-2-oxo-(9CI) synthesis
- Product Name:6-Benzoxazolesulfonylchloride,2,3-dihydro-3-methyl-2-oxo-(9CI)
- CAS Number:62522-63-8
- Molecular formula:C8H6ClNO4S
- Molecular Weight:247.66
21892-80-8
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62522-63-8
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$117.00/250mg
Yield:62522-63-8 91%
Reaction Conditions:
with chlorosulfonic acid at 0;Inert atmosphere;Schlenk technique;Reflux;
Steps:
1.2. 3-Methylbenzoxanylinon-6-ylsulfonyl chloride
3-Methylbenzoxalinone (2) (0.600 g, 4.02 mmol) was added to chlorosulfonic acid (2.343 g,20.1 mmol) in small portions at 0 oC. Then, the reaction mixture was heated to 60 oC for 2 h withstirring. The reaction mixture was cooled to room temperature, and slowly poured into crushed ice toform precipitate. The resulting precipitate was collected by filtration. The solid was dissolved in EtOAcand the organic layer was washed with water, brine, dried over MgSO4, and concentrated in vacuo toafford 3 as a light brown solid (0.903 g, 91%): 1H NMR (300 MHz, CDCl3) δ 7.99 (dd, J = 8.4, 1.8 Hz,1H), 7.89 (d, J = 1.6 Hz, 1H), 7.17 (d, J = 8.4 Hz, 1H), 3.52 (s, 3H). The data were consistent withliterature values.
References:
Zhou, Yuchen;McGillick, Brian E.;Teng, Yu-Han Gary;Haranahalli, Krupanandan;Ojima, Iwao;Swaminathan, Subramanyam;Rizzo, Robert C. [Bioorganic and Medicinal Chemistry,2016,vol. 24,# 20,p. 4875 - 4889] Location in patent:supporting information
59-49-4
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62522-63-8
59 suppliers
$117.00/250mg
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62522-63-8
59 suppliers
$117.00/250mg