ETHYL 5-(CHLOROSULFONYL)-3-FUROATE synthesis
- Product Name:ETHYL 5-(CHLOROSULFONYL)-3-FUROATE
- CAS Number:256373-91-8
- Molecular formula:C7H7ClO5S
- Molecular Weight:238.65
614-98-2
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7791-25-5
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256373-91-8
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Yield:256373-91-8 90 %
Reaction Conditions:
with pyridine;phosphorus pentachloride
Steps:
2 Step 2:
Step 2:
Ethyl furan-2-sulfonyl chloride-4-formate (2c)
Compound 2b (22.00 g, 0.157 mol) was dissolved in DCM (250 mL) at room temperature, and the solution was cooled to -15 °C in an ice salt bath.
Sulfonyl chloride (23.31 g, 0.173 mol) was added dropwise slowly while controlling the temperature to be not higher than -10 °C.
After dropwise addition was completed, the reaction system was reacted for 12 h at room temperature and cooled to -15 °C or lower in an ice salt bath.
Pyridine (13.66 g, 0.173 mol) was added dropwise slowly, and then phosphorus pentachloride (36.00 g, 0.137 mol) was added in batches while controlling the temperature to be not higher than -10 °C.
After the addition was completed, the reaction system was reacted for 2 h at room temperature.
After the reaction was completed as detected by TLC, the reaction system was added into ice water (200 mL) to quench the reaction, and then extracted with EA (200 mL * 3).
The organic phases were combined, washed with saturated brine (100 mL), dried over anhydrous sodium sulfate and concentrated under reduced pressure to remove the solvent, so as to give compound 2c in the form of a brown oil (33.00 g, 90% yield), which was directly used in the next step without purification.
References:
EP4059930,2022,A1
614-98-2
155 suppliers
$12.00/1g
256373-91-8
25 suppliers
$210.25/1g
256373-92-9
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256373-91-8
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$210.25/1g
488-93-7
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$5.00/250mg
256373-91-8
25 suppliers
$210.25/1g