Methyl malonyl chloride → HCID 86682941、化合物
反応式
Cl[C:2](=[O:8])[CH2:3][C:4]([O:6][CH3:7])=[O:5].[NH2:9][C:10]1[C:15]([Cl:16])=[CH:14][C:13]([Cl:17])=[CH:12][C:11]=1[C:18]([C:20]1[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=1)=[O:19]>C(Cl)Cl>[CH3:7][O:6][C:4](=[O:5])[CH2:3][C:2]([NH:9][C:10]1[C:15]([Cl:16])=[CH:14][C:13]([Cl:17])=[CH:12][C:11]=1[C:18](=[O:19])[C:20]1[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=1)=[O:8]参加物
4
実験手順
Methyl 3-chloro-3-oxopropanoate (317 mg, 249 μl, 2.25 mmol, Eq: 1.2) was added dropwise to a yellow solution of (2-amino-3,5-dichloro-phenyl)-phenyl-methanone (500 mg, 1.88 mmol, Eq: 1.00) in DCM (5 ml) at 0° C. The yellow solution was then allowed to warm slowly to RT. After completion of the reaction the mixture was washed with sat. NaHCO3 solution and brine, dried with Na2SO4 and evaporated. The remaining light brown residue (603 mg) was used in the next reaction step without further purification. MS (ESI): 366.0 (M+H)+.
後処理
- customAfter completion of the reaction the mixture
- washwas washed with sat. NaHCO3 solution and brine
- dry with materialdried with Na2SO4
- customevaporated
- customThe remaining light brown residue (603 mg) was used in the next reaction step without further purification
出典と根拠
- ORDレコード
- ord-998d4d5658704a9da0232698b0de309b
- 出典データセット
- uspto-grants-2015_12
- 特許番号
- US09199938B2
反応ノート
読み込み中…