Diethyl Ether → HCID 13631104、化合物
反応式
[O:1]=[C:2]1[CH2:5][CH2:4][N:3]1[CH2:6][C:7]([O:9]CC)=O.O.[NH3:13].C(Cl)(Cl)Cl.CCOCC>CO>[O:1]=[C:2]1[CH2:5][CH2:4][N:3]1[CH2:6][C:7]([NH2:13])=[O:9]参加物
6
実験手順
In 0.8 ml of methanol was dissolved 843 mg of compound (19) and 0.4 ml of conc. ammonia water was added to the solution under ice cooling followed by stirring at room temperature for 18 hours. The reaction mixture was concentrated under reduced pressure. The residue was purified by column chromatography (30 g of silica gel, chloroform-methanol=10:1) to obtain 550 mg of a roughly purified product. The product was treated with a solvent mixture of 3 ml of chloroform and 3 ml of ether to crystallize. Thus 360 mg of α-(2-oxo-1-azetidinyl)acetamide (22) was obtained as colorless crystals.
後処理
- additionwas added to the solution under ice cooling
- concentrationThe reaction mixture was concentrated under reduced pressure
- customThe residue was purified by column chromatography (30 g of silica gel, chloroform-methanol=10:1)
- customto obtain 550 mg of a roughly purified product
- customto crystallize
出典と根拠
- ORDレコード
- ord-58eab94efa0847459be40573bd5bc63d
- 出典データセット
- uspto-grants-1988_01
- 特許番号
- US04719207
反応ノート
読み込み中…