Acetone → 1-(3-Chloro-1-methyl-5,6,7,8-tetrahydroisoquinolin-4-yl)-but-1-en-3-one
反応式
[Cl:1][C:2]1[N:3]=[C:4]([CH3:14])[C:5]2[CH2:6][CH2:7][CH2:8][CH2:9][C:10]=2[C:11]=1[CH:12]=O.[OH-].[Na+].O.[CH3:18][C:19]([CH3:21])=[O:20]>>[Cl:1][C:2]1[N:3]=[C:4]([CH3:14])[C:5]2[CH2:6][CH2:7][CH2:8][CH2:9][C:10]=2[C:11]=1[CH:12]=[CH:18][C:19](=[O:20])[CH3:21]参加物
5
実験手順
3-Chloro-1-methyl-5,6,7,8-tetrahydroisoquinoline-4-carboxaldehyde (4.0 g) was stirred with a few drops of a 2% aqueous sodium hydroxide solution in aqueous acetone (1:2 v/v; 20 ml) at room temperature for 4 hr. the mixture was poured into water which was then extracted with the diethyl ether. The residue obtained after evaporation of the dried (MgSO4) organic extract was purified by column chromatography over silica with dichloromethane elution to give 1-(3-chloro-1-methyl-5,6,7,8-tetrahydroisoquinolin-4-yl)-but-1-en-3-one as white crystals, mp 90° C.
後処理
- extractionwas then extracted with the diethyl ether
- customThe residue obtained
- customafter evaporation of the
- dry with materialdried (MgSO4)
- extractionorganic extract
- customwas purified by column chromatography over silica with dichloromethane elution
出典と根拠
- ORDレコード
- ord-ab9f6f05c203449c8d039107e6e16a03
- 出典データセット
- uspto-grants-1987_07
- 特許番号
- US04680400
反応ノート
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