反応式
[O:1]1[C:7]2[CH:8]=[CH:9][CH:10]=[CH:11][C:6]=2[NH:5][CH2:4][CH2:3][CH2:2]1.[N:12]([O-])=[O:13].[Na+]>Cl.O>[N:12]([N:5]1[C:6]2[CH:11]=[CH:10][CH:9]=[CH:8][C:7]=2[O:1][CH2:2][CH2:3][CH2:4]1)=[O:13]参加物
5
実験手順
To a stirred, cold slurry of 2,3,4,5-tetrahydro-1,5-benzoxazepine (13.72 g, 91.96 mmol) in 2N aqueous HCl (105 mL) was added dropwise a solution of NaNO2 (7.30 g, 105.75 mmol) in H2O (16 mL) and stirred at room temperature for 2 hrs. The mixture was taken up in H2O (800 mL), extracted with ether (3×200 mL), dried over MgSO4, and stripped of the solvent under reduced pressure to yield 15.59 g (95%) of 5-nitroso-2,3,4,5-tetrahydro-1,5-benzoxazepine as a tan powder. (M+H)+ 178.
後処理
- extractionextracted with ether (3×200 mL)
- dry with materialdried over MgSO4
出典と根拠
- ORDレコード
- ord-54e9657d3fcb4bd3becb32aee40351a7
- 出典データセット
- uspto-grants-2004_03
- 特許番号
- US06713471B1
関連ノート
読み込み中…