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HRID 1040642作成日:2026年10月27日

Dimethylformamide → 8-Methoxy-2-methyl-2,3,4,5-tetrahydro-benzo[c]azepin-1-one

https://huagongshe.com/reaction/1040642

反応式

関与物質

役割名称HCID仕込み量
反応物DimethylformamideHCID 6228—
反応物Sodium hydrideHCID 24758—
反応物8-Methoxy-2,3,4,5-tetrahydro-benzo[c]azepin-1-oneHCID 11275529—
生成物8-Methoxy-2-methyl-2,3,4,5-tetrahydro-benzo[c]azepin-1-oneHCID 67264562—

反応手順

A mixture of 8-Methoxy-2,3,4,5-tetrahydro-benzo[c]azepin-1-one (283 mgs, 1.48 mmol) in DMF (5 mL) was treated with NaH (60% dispersion in mineral oil, 75 mgs, 1.85 mmol) and stirred for 10 min. The mixture was quenched with water and extracted with ether. The organic layers were washed with brine and the organic layer dried (MgSO4), filtered and concentrated to give 8-Methoxy-2-methyl-2,3,4,5-tetrahydro-benzo[c]azepin-1-one (227 mgs). 1H-NMR (CDCl3) δ 7.14 (d, J=2.7 Hz, 1H), 6.96 (d, J=8.1 Hz, 1H), 6.83-6.81 (m, 1H), 3.74 (s, 3H), 3.14 (t, J=6.6 Hz, 2H), 3.10 (s, 3H), 2.64 (t, J=8.1 Hz, 2H), 1.97-1.91 (m, 2H); LC/MS (ESI+): 273 (M+H).

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US08552186B2
出典データセットuspto-grants-2013_10
ORD IDord-e51a1c56b3584e009df86d8bad6ae1cd
出典メモuspto-grants-2013_10