Water → HCID 67549266、化合物
反応式
C([O:3][C:4](=O)[CH2:5][N:6]1[CH2:11][CH2:10][O:9][CH2:8][C:7]1=[O:12])C.O.[NH2:15][NH2:16].O>C(O)C>[O:12]=[C:7]1[N:6]([CH2:5][C:4]([NH:15][NH2:16])=[O:3])[CH2:11][CH2:10][O:9][CH2:8]1参加物
5
反応条件
- 温度
- 80 °C
実験手順
Ethyl-2-(3-oxomorpholino)acetate (600 mg, 3.21 mmol) was dissolved in ethanol (3 mL) and hydrazine hydrate (160.46 mg, 3.21 mmol) was added at room temperature. The reaction mixture was heated at 80° C. for 1 h. The reaction mixture was transferred into 50 mL water and extracted with EtOAc (3×50 mL). The combined organic layers was washed with brine, dried over anhydrous sodium sulphate, and concentrated under reduced pressure to give the crude product, which was used without further purification in the subsequent step (Crude yield: 54%). LCMS m/z 174.05 [M+H]+ tR 2.489 min.
後処理
- extractionextracted with EtOAc (3×50 mL)
- washThe combined organic layers was washed with brine
- dry with materialdried over anhydrous sodium sulphate
- concentrationconcentrated under reduced pressure
出典と根拠
- ORDレコード
- ord-8e001fc63f9742d8b3db035798c11a5c
- 出典データセット
- uspto-grants-2016_02
- 特許番号
- US09266843B2
反応ノート
読み込み中…