Ammonium Acetate → tert-Butyl ((2S,3S)-2-methyl-4-oxoazetidin-3-yl)carbamate
反応式
[C:1]([O:5][C:6]([NH:8][C@H:9]1[C@H:12]([CH3:13])[N:11](O)[C:10]1=[O:15])=[O:7])([CH3:4])([CH3:3])[CH3:2].C([O-])(=O)C.[NH4+]>CO.[Cl-].[Na+].[Cl-].[Cl-].[Cl-].[Ti+3]>[C:1]([O:5][C:6]([NH:8][C@H:9]1[C@H:12]([CH3:13])[NH:11][C:10]1=[O:15])=[O:7])([CH3:4])([CH3:2])[CH3:3]参加物
6
実験手順
A solution of 4.98 of (3S-trans)-3-t-butoxycarbonylamino-1-hydroxy-4-methylazetidinone in 200 ml of methanol is treated with 132 ml of 4.5M ammonium acetate and then 66 ml of 1.5M titanium trichloride and stirred for 4.5 hours. The aqueous solution is diluted with an equal volume of 8% sodium chloride and extracted with ethyl acetate to give 3.48 g of crude product. Recrystallization from ether-hexane yields 3.3 g of the title compound.
後処理
- extractionextracted with ethyl acetate
- customto give 3.48 g of crude product
- customRecrystallization from ether-hexane
出典と根拠
- ORDレコード
- ord-73b3ea52cda147bb886fa1ce3731902e
- 出典データセット
- uspto-grants-1988_10
- 特許番号
- US04775670
反応ノート
読み込み中…