Hydrochloric Acid → HCID 11522579、化合物
反応式
[ClH:1].Cl.[CH3:3][N:4]([CH2:6][CH:7]1[CH2:15][C:14]2[C:9](=[CH:10][CH:11]=[C:12]([O:16][CH3:17])[CH:13]=2)[C:8]1([C:19]1[CH:20]=[N:21][CH:22]=[CH:23][CH:24]=1)O)[CH3:5]>>[ClH:1].[CH3:17][O:16][C:12]1[CH:13]=[C:14]2[C:9]([C:8]([C:19]3[CH:20]=[N:21][CH:22]=[CH:23][CH:24]=3)=[C:7]([CH2:6][N:4]([CH3:5])[CH3:3])[CH2:15]2)=[CH:10][CH:11]=1参加物
3
実験手順
About 9 ml of 37% hydrochloric acid were added at room temperature to 0.837 g of 2-dimethylaminomethyl-5-methoxy-1-pyridin-3-yl-indan-1-ol hydrochloride (mixture of the diastereoisomers); the mixture was stirred overnight and then concentrated in vacuo at 70° C. The residue was taken up twice in dichloromethane and concentrated again. The oily brown residue was taken up in 40 ml of acetone and stirred, whereupon a crystalline solid formed. After further stirring for 2.5 days, filtration with suction was carried out with the exclusion of air, followed by washing twice with diethyl ether and drying under an oil-pump vacuum. 0.603 g of (6-methoxy-3-pyridin-3-yl-1H-inden-2-ylmethyl)-dimethyl-amine hydrochloride was obtained.
後処理
- additionmixture of the diastereoisomers)
- concentrationconcentrated in vacuo at 70° C
- concentrationconcentrated again