Sodium Hydroxide → 1-Isopropyl-5-dichloroacetylaminomethylisoquinoline
反応式
[C:1]([NH:9][CH2:10][CH2:11][C:12]1[CH:17]=[CH:16][CH:15]=[CH:14][C:13]=1Cl)(=O)[C:2]1[CH:7]=CC=C[CH:3]=1.C(C1C2C(=CC=CC=2)C=CN=1)(C)C.O[CH2:33][NH:34][C:35](=[O:39])[CH:36]([Cl:38])[Cl:37].[OH-].[Na+]>S(=O)(=O)(O)O.O>[CH:2]([C:1]1[C:13]2[C:12](=[C:17]([CH2:33][NH:34][C:35](=[O:39])[CH:36]([Cl:38])[Cl:37])[CH:16]=[CH:15][CH:14]=2)[CH:11]=[CH:10][N:9]=1)([CH3:3])[CH3:7]参加物
実験手順
(a-2-2) Ten grams of 1-(1-benzoyloxy-1-methylethyl)-isoquinoline was dissolved in 100 ml of ethanol, and 2 g of 10% palladium-carbon was dissolved. The mixture was stirred in a stream of hydrogen at room temperature and atmospheric pressure for 24 hours. The reaction mixture was filtered through Celite, and the solvent was distilled off. Distillation under reduced pressure afforded 4.0 g of 1-isopropylisoquinoline. (b) A mixture of 9.4 g of 1-isopropylisoquinoline and 12 g of N-hydroxymethyl dichloroacetamide was dissolved in 94 g of conc. sulfuric acid and 9.5 g of 20% fuming sulfuric acid, and the solution was heated for 3 hours. The reaction mixture was poured into water, made weakly alkaline with an aqueous solution of sodium hydroxide, and extracted with ethyl acetate. The solvent was distilled off, and the residue was recrystallized from ethyl acetate-benzene to afford 20 g of 1-isopropyl-5-dichloroacetylaminomethylisoquinoline having a melting point of 150.7° to 151.0° C.
後処理
- extractionextracted with ethyl acetate
- distillationThe solvent was distilled off
- customthe residue was recrystallized from ethyl acetate-benzene
出典と根拠
- ORDレコード
- ord-18cf2404fe6d4bf0b4fe6f350f652c7f
- 出典データセット
- uspto-grants-1982_06
- 特許番号
- US04337256
反応ノート
読み込み中…