3-ACETYL-2,3,4,5-TETRAHYDRO-1H-BENZO[D]AZEPINE-7-SULFONYL CHLORIDE synthesis
- Product Name:3-ACETYL-2,3,4,5-TETRAHYDRO-1H-BENZO[D]AZEPINE-7-SULFONYL CHLORIDE
- CAS Number:35760-18-0
- Molecular formula:C12H14ClNO3S
- Molecular Weight:287.76
10533-22-9
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35760-18-0
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Yield:35760-18-0 45%
Reaction Conditions:
with chlorosulfonic acid in dichloromethane;water;
Steps:
3-Acetyl-7-chlorosulfonyl-2,3,4,5-tetrahydro-1H-3-benzazepine
3-Acetyl-7-chlorosulfonyl-2,3,4,5-tetrahydro-1H-3-benzazepine A solution of 3-acetyl-2,3,4,5-tetrahydro-1H-3-benzazepine (4.0 g, 0.021 mol) in dichloromethane (25 ml) was added dropwise to a stirred solution of chlorosulphonic acid in dichloromethane (25 ml) at -70° C. under argon. After warming to room temperature, the reaction was stirred for 18 h before being quenched in ice/water (200 ml). The resulting mixture was extracted with ethyl acetate (3*100 ml), dried (Na2SO4) and the solvent evaporated in vacuo to give the title compound (2.74 g, 45%) as a pale yellow solid. 1H NMR: δ (CDCl3): 2.21 (3H, s), 3.0-3.10 (4H, m), 3.60-3.70 (2H, m), 3.74-3.80 (2H, m), 7.35-7.40 (1H, m), 7.80-7.85 (2H, m). Mass spectrum AP+: Found 288 & 290 (MH+). C12H14NSO2Cl requires 287 & 289.
References:
US2004/171606,2004,A1
613-73-0
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$22.80/5g
35760-18-0
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4424-20-8
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$49.00/100mg
35760-18-0
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