Benzaldehyde → HCID 58696280、化合物
反応式
C(N(CC)CC)C.[CH:8](=O)[C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=1.Cl.[NH2:17][CH:18]([C:24]1[CH:29]=[CH:28][C:27]([Cl:30])=[C:26]([Cl:31])[CH:25]=1)[C:19]([O:21][CH2:22][CH3:23])=[O:20]>C(#N)C>[CH2:22]([O:21][C:19](=[O:20])[CH:18]([N:17]=[CH:8][C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=1)[C:24]1[CH:29]=[CH:28][C:27]([Cl:30])=[C:26]([Cl:31])[CH:25]=1)[CH3:23]参加物
5
実験手順
Triethylamine (170 mL) and benzaldehyde (130 mL) were added to a suspension of ethyl amino-(3,4-dichlorophenyl)-acetate hydrochloride (350 g) in acetonitrile (1.5 L), followed by stirring at room temperature overnight. The insoluble matter was removed through Celite, followed by washing with ethyl acetate. The filtrate was subjected to partitioning with water and then extraction with ethyl acetate. The thus-obtained organic layer was washed with saturated brine, and then dried over sodium sulfate anhydrate. The solvent was removed under reduced pressure, to thereby give the title compound (425 g). The title compound was used in the next step without further purification.
後処理
- customThe insoluble matter was removed through Celite
- washby washing with ethyl acetate
- customto partitioning with water
- extractionextraction with ethyl acetate
- washThe thus-obtained organic layer was washed with saturated brine
- dry with materialdried over sodium sulfate anhydrate
- customThe solvent was removed under reduced pressure
出典と根拠
- ORDレコード
- ord-05cd4704ccac4b3185bf5dea055323e5
- 出典データセット
- uspto-grants-2007_10
- 特許番号
- US07276511B2
反応ノート
読み込み中…