7-hydroxy-4,5-dihydro-1H-benzo[b]azepin-2(3H)-one synthesis
- Product Name:7-hydroxy-4,5-dihydro-1H-benzo[b]azepin-2(3H)-one
- CAS Number:22245-90-5
- Molecular formula:C10H11NO2
- Molecular Weight:177.2
1312005-59-6
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22245-90-5
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Yield:22245-90-5 64%
Reaction Conditions:
with dihydrogen peroxide;sodium hydroxide in tetrahydrofuran at 20; for 2 h;
Steps:
14.2 Step 2: 7-phenolic hydroxy-1,3,4,5-tetrahydro-2H-benzo[b]azepin-2-one
The compound 7- (4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl) -1,3,4,5-tetrahydro-2H-benzo [ B) azza-2-one (1 g, 3.48 mmol) was dissolved in tetrahydrofuran (20 mL)Has added hydrogen peroxide (10mL, 36%),Sodium hydroxide solution (7 mL, 1 N),Reaction at room temperature for 2 hours,The reaction was terminated by the addition of saturated sodium bisulfite solution (5 g dissolved in 10 mL of water)The mixture was adjusted to pH 4 with 2N sodium hydroxide.After extraction with ethyl acetate, the organic layer was washed with brine, dried and concentrated. The crude product was separated by column chromatography (dichloromethane / methanol from 100: 0 to 90:10, v / v) to give 7-phenolic hydroxyl- 4,5-tetrahydro-2H-benzo [b] azepan-2-one(0.4 g) in 64% yield.
References:
CN106349241,2017,A Location in patent:Paragraph 0313; 0317; 0318; 0319
4424-80-0
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![7-BROMO-1,3,4,5-TETRAHYDRO-BENZO[B]AZEPIN-2-ONE](/CAS/GIF/53841-99-9.gif)
53841-99-9
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22245-90-5
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