3-OXO-3,4-DIHYDRO-2H-1,4-BENZOXAZINE-6-SULFONYL CHLORIDE synthesis
- Product Name:3-OXO-3,4-DIHYDRO-2H-1,4-BENZOXAZINE-6-SULFONYL CHLORIDE
- CAS Number:31794-45-3
- Molecular formula:C8H6ClNO4S
- Molecular Weight:247.66
5466-88-6
199 suppliers
$25.00/5g
31794-45-3
62 suppliers
$45.00/250 mg
Yield:31794-45-3 66%
Reaction Conditions:
with chlorosulfonic acid at 0 - 10; for 1.33333 h;
Steps:
8 Synthesis of 3-oxo-3,4-dihydro-2H-benzo[b][1,4]oxazine-6-sulfonyl Chloride
Synthesis of 3-oxo-3,4-dihydro-2H-benzo[b][1,4]oxazine-6-sulfonyl Chloride Into a 100 mL round-bottom flask, was placed HSO3Cl (10 mL). To the above was added 2H-benzo[b][1,4]oxazin-3(4H)-one (2 g, 13.42 mmol) in several batches, while cooling to a temperature of 0-5° C. over a time period of 20 min. The resulting solution was allowed to react, with stirring, for 1 h while the temperature was maintained at 5-10° C. The reaction mixture was poured into 100 g of ice carefully. The resulting solution was extracted one time with 100 mL of CH2Cl2 and the organic layers combined and dried over Na2SO4. A filtration was performed. The filtrate was concentrated by evaporation under vacuum using a rotary evaporator. This resulted in 2.2 g (66%) of 3-oxo-3,4-dihydro-2H-benzo[b][1,4]oxazine-6-sulfonyl chloride as a white solid. 1H NMR (400 MHz, CDCl3, δ) 9.29 (s, 1H), 7.71 (d, 2H), 7.52 (s, 1H), 7.16 (d, 2H), 4.80 (s, 2H). ES-MS m/z 317 [M+BnNH-H]
References:
MEMORY PHARMACEUTICALS CORPORATION US2008/318941, 2008, A1 Location in patent:Page/Page column 26
95-55-6
553 suppliers
$5.00/5 g
31794-45-3
62 suppliers
$45.00/250 mg
89976-75-0
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$19.00/100mg
31794-45-3
62 suppliers
$45.00/250 mg