3-IODO-BENZAZEPIN-2-ONE synthesis
- Product Name:3-IODO-BENZAZEPIN-2-ONE
- CAS Number:140700-64-7
- Molecular formula:C10H10INO
- Molecular Weight:287.1
4424-80-0
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Yield:140700-64-7 96%
Reaction Conditions:
with trimethylsilyl iodide;N,N,N,N,-tetramethylethylenediamine;iodine in dichloromethane;
Steps:
4.19.A 1-[[3-[[2,2-Dicyano-1-[(2-methyl-5-benzofuranyl)amino]ethenyl]amino]-2,3,4,5-tetrahydro-2-oxo-1H-1-benzazepin-1-yl]acetyl]pyrrolidine
A. Preparation of 3-iodo-1,3,4,5-tetrahydro-2H-1-benzazepin-2-one. Trimethylsilyl iodide (0.56 mL, 0.4 mmol) was added to a solution of 1,3,4,5-tetrahydro-2H-1-benzazepin-2-one (0.32 g, 2.0 mmol) and TMEDA (0.91 mL, 6.0 mmol) in dichloromethane (10 mL) stirring at -15° C. After stirring at -15° C. for 15 min, iodine (0.76 g, 3.0 mmol) was added. The reaction was allowed to warm to 0°0C. and was stirred for 2 h. The reaction mixture was transferred to a separatory funnel and washed with 1/1 10% Na2SO3/brine, dried with sodium sulfate, and evaporated to afford 0.94 g of crude product. Chromatography (silica, 25% ethyl acetate/hexane) gave 3-iodo-1,3,4,5-tetrahydro-2H-1-benzazepin-2-one (0.55 g, 96% yield): 1H-NMR (CDCl3) δ 7.32-7.16 (m, 3 H), 6.99 (m, 1 H), 4.68 (m, 1 H), 2.99 (m, 1 H), 2.82-2.65 (m, 3 H).
References:
US2002/25957,2002,A1
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