1-methyl-3,4-dihydro-1H-benzo[b]azepin-5(2H)-one synthesis
- Product Name:1-methyl-3,4-dihydro-1H-benzo[b]azepin-5(2H)-one
- CAS Number:3749-11-9
- Molecular formula:C11H13NO
- Molecular Weight:175.23
![1,2,3,4-Tetrahydro-benzo[b]azepin-5-one](/CAS/GIF/1127-74-8.gif)
Yield:3749-11-9 91.9 %
Reaction Conditions:
with sodium tris(acetoxy)borohydride;acetic acid in 1,2-dichloro-ethane at 20;
Steps:
1-Methyl-1,2,3,4-tetrahydro-5H-benzo[b]azepin-5-one (G-1):
A mixture of 2,3,4,5-tetrahydro-1H-1-benzazepin-5-one (2.0 g, 12.4 mmol), paraformaldehyde (4.1 g, 45.8 mmol), NaBH(OAc)3 (9.7 g, 45.8 mmol) and acetic acid (744 mg, 12.4 mmol) in DCE (40 mL) was stirred at room temperature for 16 hours. Saturated NaHCO3 (60 mL) was added to above reaction solution, the resulting mixture was stirred 30 min at 0 °C and then extracted with DCM (60 mL* 2). The combined organic layers were washed with brine (80 mL), dried over sodium sulfate, filtered and concentrated to dryness. The residue was purified by column chromatography (eluted with petroleum ether: ethyl acetate = 10: 1) to obtain the desired product (2.0 g, 91.9% yield) as a yellow oil. MS(ESI) calculated for C11H13NO, 175.1; found 176.1
References:
WO2022/204150,2022,A1 Location in patent:Paragraph 0239
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