Hydrazine → HCID 178451520、化合物
反応式
[NH2:1]N.C[N:4](/[CH:6]=[C:7]1/[CH2:8][N:9]([C:13]([O:15][C:16]([CH3:19])([CH3:18])[CH3:17])=[O:14])[CH2:10][C:11]/1=O)C>C(O)C>[N:1]1[NH:4][CH:6]=[C:7]2[CH2:8][N:9]([C:13]([O:15][C:16]([CH3:19])([CH3:18])[CH3:17])=[O:14])[CH2:10][C:11]=12参加物
4
実験手順
A solution of hydrazine (3 mL) and tert-butyl(3Z)-3-[(dimethylamino)methylene]-4-oxopyrrolidine-1-carboxylate (19.22 g) in ethanol (40 mL) was heated at 85° C. in a sealed tube for 4 h. Solvent was removed under reduced pressure, and the residue was triturated with dichloromethane (160 mL) and ethyl acetate (15 mL). The resulting solid was filtered. The filtrate was concentrated and the resulting solid was triturated again and filtered. The combined solids were used without further purification. LC/MS: 210.1 (M+1).
後処理
- customSolvent was removed under reduced pressure
- customthe residue was triturated with dichloromethane (160 mL) and ethyl acetate (15 mL)
- filtrationThe resulting solid was filtered
- concentrationThe filtrate was concentrated
- customthe resulting solid was triturated again
- filtrationfiltered
- customThe combined solids were used without further purification
出典と根拠
- ORDレコード
- ord-b5cb201186a94c27860b15b7b34c87ae
- 出典データセット
- uspto-grants-2015_03
- 特許番号
- US08980929B2
反応ノート
読み込み中…