反応式
Br[CH:2]([CH3:12])[C:3]([C:5]1[CH:10]=[CH:9][CH:8]=[C:7]([Cl:11])[CH:6]=1)=[O:4].[NH2:13][C:14]([CH3:18])([CH3:17])[CH2:15][OH:16]>CO>[Cl:11][C:7]1[CH:6]=[C:5]([C@@:3]2([OH:4])[O:16][CH2:15][C:14]([CH3:18])([CH3:17])[NH:13][C@@H:2]2[CH3:12])[CH:10]=[CH:9][CH:8]=1参加物
実験手順
To a solution of 2-bromo-3′-chloropropiophenone (19.3 g, 0.08 mol) in MeOH (100 mL) was added dropwise a solution of 2-amino-2-methyl-1-propanol (27.8 g, 0.31 mol) in methanol (200 mL) at ambient temperature. The mixture was stirred for 18 h and concentrated in vacuo. The residue was partitioned between water and diethyl ether. The combined organic phase was extracted with 10% aqueous hydrogen chloride. The combined aqueous acid extracts were chilled in an ice bath and made basic with 40% aqueous sodium hydroxide. The mixture was extracted with diethyl ether, the combined diethyl ether extracts were washed with water and saturated sodium chloride solution, dried (K2CO3) and concentrated in vacuo to give 15.0 g (75%) of (+/−)-(2R*,3R*)-2-(3-chlorophenyl)-3,5,5-trimethyl-2-morpholinol as an off-white solid.
後処理
- concentrationconcentrated in vacuo
- customThe residue was partitioned between water and diethyl ether
- extractionThe combined organic phase was extracted with 10% aqueous hydrogen chloride
- temperatureThe combined aqueous acid extracts were chilled in an ice bath
- extractionThe mixture was extracted with diethyl ether
- washthe combined diethyl ether extracts were washed with water and saturated sodium chloride solution
- dry with materialdried (K2CO3)
- concentrationconcentrated in vacuo
出典と根拠
- ORDレコード
- ord-f445d616aec14a1cadaf75885a501d9d
- 出典データセット
- uspto-grants-2006_02
- 特許番号
- US06998400B2
関連ノート
読み込み中…