反応式
[CH2:1]([C:5]12[CH2:17][CH2:16][C:15](=O)[C:14]([CH3:19])=[C:13]1[C:12]1[C:7](=[CH:8][C:9]([OH:20])=[CH:10][CH:11]=1)[CH2:6]2)[CH2:2][CH2:3][CH3:4].Cl.[OH:22][NH2:23]>N1C=CC=CC=1>[CH2:1]([C:5]12[CH2:17][CH2:16]/[C:15](=[N:23]\[OH:22])/[C:14]([CH3:19])=[C:13]1[C:12]1[C:7](=[CH:8][C:9]([OH:20])=[CH:10][CH:11]=1)[CH2:6]2)[CH2:2][CH2:3][CH3:4]参加物
4
反応条件
- 温度
- 60 °C
実験手順
A solution of 9a-butyl-7-hydroxy-4-methyl-1,2,9,9a-tetrahydro-3H-fluoren-3-one (60 mg, 0.22 mmol) and hydroxyl amine hydrochloride (77 mg, 1.11 mmol) in anhydrous pyridine (0.5 mL) was stirred under a nitrogen atmosphere at room temperature for 4.3 hours and then heated in an oil bath at 60° C. for 30 minutes. The reaction mixture was evaporated under vacuum to an oil which was taken up in EtOAc (10 mL), washed with 1N HCl (2×6 ml), water (6 mL) and brine (6 ml), dried over MgSO4, filtered, and evaporated under vacuum. The residue was lyophilized from benzene (3 mL) to afford (3E)-9a-butyl-7-hydroxy-4-methyl-1,2,9,9a-tetrahydro-3H-fluoren-3-one oxime as an amorphous solid.
後処理
- customThe reaction mixture was evaporated under vacuum to an oil which
- washwashed with 1N HCl (2×6 ml), water (6 mL) and brine (6 ml)
- dry with materialdried over MgSO4
- filtrationfiltered
- customevaporated under vacuum
出典と根拠
- ORDレコード
- ord-939af69376254c7286149b31bfef6201
- 出典データセット
- uspto-grants-2006_08
- 特許番号
- US07087599B2
関連ノート
読み込み中…