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CAS No. : | 402-46-0 | MDL No. : | MFCD00025384 |
Formula : | C6H6FNO2S | Boiling Point : | - |
Linear Structure Formula : | - | InChI Key : | LFLSATHZMYYIAQ-UHFFFAOYSA-N |
M.W : | 175.18 | Pubchem ID : | 120231 |
Synonyms : |
|
Signal Word: | Warning | Class: | |
Precautionary Statements: | P301+P312+P330-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 |
---|---|---|
41% | With caesium carbonate; In dimethyl sulfoxide; at 168℃;Inert atmosphere; | A round bottom flask was charged with 4-fluorobenzenesulfonamide (945 mg, 5.4 mmol), L-proline-t-butyl ester HCl (1.24 g, 6 mmol), and cesium carbonate (4.2 g, 12 mmol) and suspended in 10 ml anhydrous DMSO. The mixture was placed in a preheated oil bath and equipped with a condenser, and heated under nitrogen at 168 oC overnight. HPLC analysis of the mixture indicated complete conversion of the benzenesulfonamide starting material. The mixture was transferred to an Erlenmeyer flask, the reaction pot was diluted with 2 ml of concentrated HCl, and added to the mixture in the Erlenmeyer flask and allowed to stir. The aqueous was then extracted with ethyl acetate (3 x 50 ml), and the combined extracts were washed with water (3 x 15 ml). The volatiles were then removed under vacuum, and 1.24 g of crude material was obtained. The desired intermediate was isolated using MPLC, utilizing a 0 to 60% gradient of acetone in DCM, affording 0.56 g (41%):1H NMR (300 MHz, DMSO-d6)d ppm 7.58 (d, J= 9.0 Hz, 2H), 6.98 (s, 2H), 6.54 (d, J= 9.0 Hz, 2H), 4.28 (d, J= 8.4 Hz, 1H), 2.35-2.22 (m, 2H), 2.04-1.96 (m, 2H). |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
With caesium carbonate; In dimethyl sulfoxide; at 168℃;Inert atmosphere; | A round bottom flaskwas charged with 4-fluorobenzenesulfonamide (945 mg, 5.4 mmol), L-proline-t-butyl ester HCl(1.24 g, 6 mmol), and cesium carbonate (4.2 g, 12 mmol) and suspended in 10 mL anhydrousDMSO. The mixture was placed in a preheated oil bath and equipped with a condenser, and10 heated under nitrogen at 168 C overnight. HPLC analysis of the mixture indicated completeconversion of the benzenesulfonamide starting material. The mixture was transferred to anErlenmeyer flask, the reaction pot was diluted with 2 mL of concentrated HCl, and added to themixture in the Erlenmeyer flask and allowed to stir. The aqueous was then extracted with ethylacetate (3 x 50 mL ), and the combined extracts were washed with water (3 x 15 mL ). The15 volatiles were then removed under vacuum, and 1.24 g of crude material was obtained. Thedesired intermediate was isolated using MPLC, utilizing a 0 to 60% gradient of acetone in DCM,affording 35 (0.56 g, 41 %): 1H NMR (300 MHz, DMSO-d6) 8 ppm 7.58 (d, J= 9.0 Hz, 2H), 6.98(s, 2H), 6.54 (d, J= 9.0 Hz, 2H), 4.28 (d, J= 8.4 Hz, 1H), 2.35-2.22 (m, 2H), 2.04-1.96 (m, 2H). |
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