Potassium Hydroxide → 2,3,4,5-Tetrahydro-1,5-benzoxazepine
反応式
[OH-].[K+].ClC[CH2:5][CH2:6][N:7]1[C:11]2[CH:12]=[CH:13][CH:14]=[CH:15][C:10]=2[O:9][C:8]1=O>C(O)CCC>[O:9]1[C:10]2[CH:15]=[CH:14][CH:13]=[CH:12][C:11]=2[NH:7][CH2:6][CH2:5][CH2:8]1参加物
4
実験手順
Powdered KOH (37.60 g, 0.67 mol) was added to a slurry of 3-(3-chloropropyl)-1,3-benzoxazol-2(3H)-one (35.75 g, 0.169 mol) in n-butanol (450 mL) under N2 gas and refluxed for 52 hours. The mixture was filtered and reduced to dryness under reduced pressure. The residue was taken up in H2O (500 mL) and extracted with ether (3×200 mL). The organic was washed with 10% HCl (2×200 mL), dried over MgSO4, and stripped of solvent under reduced pressure. Purification by flash chromatography (50% EtOAc in hexanes) yielded 13.72 g (54%) of 2,3,4,5-tetrahydro-1,5-benzoxazepine as a powder, m.p. 50-51° C. (M+H)+ 149.
後処理
- temperaturerefluxed for 52 hours
- filtrationThe mixture was filtered
- extractionextracted with ether (3×200 mL)
- washThe organic was washed with 10% HCl (2×200 mL)
- dry with materialdried over MgSO4
- customPurification by flash chromatography (50% EtOAc in hexanes)
出典と根拠
- ORDレコード
- ord-976260e899e04a89a7c17e9e744c8602
- 出典データセット
- uspto-grants-2004_03
- 特許番号
- US06713471B1
反応ノート
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