TERT-BUTYL 7-BROMO-4,5-DIHYDRO-1H-BENZO[C]AZEPINE-2(3H)-CARBOXYLATE synthesis
- Product Name:TERT-BUTYL 7-BROMO-4,5-DIHYDRO-1H-BENZO[C]AZEPINE-2(3H)-CARBOXYLATE
- CAS Number:740842-89-1
- Molecular formula:C15H20BrNO2
- Molecular Weight:326.23
Yield:740842-89-1 36%
Reaction Conditions:
with triethylamine in tetrahydrofuran at 25; for 16 h;
Steps:
26.C
Step C: TEA (537 mg, 5.3 mmol) was added to a solution of 7-bromo-2,3,4,5-tetrahydro-1H-benzo[c]azepine (400mg, 1.7 mmol) in THF (8.00 mL) at 25°C, followed by addition of Boc2O (579 mg, 5.3 mmol). The reaction mixturewas stirred at 25°C for 16 hours. The reaction mixture was concentrated in vacuum to give a crude product. Theresidue was purified by silica gel chromatography (200～300 mesh of silica gel, petroleum ether/ethyl acetate = 30/1to 10/1), to give t-butyl 7-bromo-4,5-dihydro-1H-benzo[c]azepine-2(3H)-formate (210 mg, 36% yield) as a yellowoil. MS (ESI) m/z: 270, 272 (M-56 + 1).
References:
EP3248968,2017,A1 Location in patent:Paragraph 0100
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