HCID 86723802、化合物 → 7-bromo-6-methyl-3,4-dihydro-1,4-benzoxazepin-5(2H)-one
反応式
[Br:1][C:2]1[CH:3]=[CH:4][C:5]2[O:11][CH2:10][CH2:9][N:8](CC3C=CC(OC)=CC=3)[C:7](=[O:21])[C:6]=2[C:22]=1[CH3:23]>C(O)(C(F)(F)F)=O>[Br:1][C:2]1[CH:3]=[CH:4][C:5]2[O:11][CH2:10][CH2:9][NH:8][C:7](=[O:21])[C:6]=2[C:22]=1[CH3:23]参加物
3
実験手順
A mixture of 7-bromo-4-(4-methoxybenzyl)-6-methyl-3,4-dihydro-1,4-benzoxazepin-5(2H)-one (130c, 2.8 g, 7.4 mmol) in TFA (30 mL) was refluxed for 14 hours. The reaction mixture was concentrated under vacuum. The residue was purified by column chromatography (petroleum ether/EtOAc, 3/1) to give 7-bromo-6-methyl-3,4-dihydro-1,4-benzoxazepin-5(2H)-one (7-bromo-6-methyl-3,4-dihydro-1,4-benzoxazepin-5(2H)-one (130d, 1.2 g, 63%) as a brown solid.
後処理
- temperaturewas refluxed for 14 hours
- concentrationThe reaction mixture was concentrated under vacuum
- customThe residue was purified by column chromatography (petroleum ether/EtOAc, 3/1)
出典と根拠
- ORDレコード
- ord-0f6a31b826034ecc8d1e61cbec3516ae
- 出典データセット
- uspto-grants-2015_05
- 特許番号
- US09040515B2
反応ノート
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